U.S. Geological Survey Protocol for Sample 

Collection in Response to the Deepwater 

Horizon Oil Spill, Gulf of Mexico, 2010 

Sampling Methods for Water, Sediment, Benthic 

Invertebrates, and Microorganisms in Coastal 

Environments 

This report supersedes USGS Open-File Report 2010–1191.

By Franceska D. Wilde and Stanley C. Skrobialowski

Open-File Report 2011–1098

U.S. Department of the Interior 

U.S. Geological Survey
U.S. Department of the Interior

KEN SALAZAR, Secretary

U.S. Geological Survey

Marcia K. McNutt, Director

U.S. Geological Survey, Reston, Virginia: 2011 

For product and ordering information:

World Wide Web: http://www.usgs.gov/pubprod

Telephone: 1-888-ASK-USGS

For more information on the USGS—the Federal source for science about the Earth,

its natural and living resources, natural hazards, and the environment:

World Wide Web: http://www.usgs.gov

Telephone: 1-888-ASK-USGS

Suggested citation:

Wilde, F.D. and Skrobialowski, S.C.., 2011, U.S. Geological Survey protocol for sample collection in 

response to the Deepwater Horizon oil spill, Gulf of Mexico, 2010: U.S. Geological Survey Open-File 

Report 2011–1098, 178 p. (Supersedes USGS Open-File Report 2010–1191.)

Any use of trade, product, or firm names is for descriptive purposes only and does not imply 

endorsement by the U.S. Government.

Although this report is in the public domain, permission must be secured from the individual 

copyright owners to reproduce any copyrighted material contained within this report.
iii

Contents

Acknowledgments........................................................................................................................ viii

1.0 Development of the Post-Landfall Sampling Protocol ............................................................. 1

1.1 Background .......................................................................................................................... 3

1.2 Objective and Approach ....................................................................................................... 3

1.3 Purpose and Scope ................................................................................................................ 4

2.0 Preparations for Sampling at Oil-Contaminated Sites .............................................................. 6

2.1 Communication with Incident Command ............................................................................ 6

2.2 Training and Safety .............................................................................................................. 6

2.3 Equipment and Supplies ....................................................................................................... 7

2.4 Prepare for Field Deployment .............................................................................................. 8

2.5 Initial Onsite Preparations .................................................................................................... 8

3.0 Safety in Field Activities ........................................................................................................ 11

3.1 Health and Safety Plans ...................................................................................................... 12

3.2 Training .............................................................................................................................. 14

3.2.1 HazWOper and British Petroleum Training .............................................................. 14

3.2.2. Motorboat Operation ................................................................................................. 15

3.2.3 Water-Quality Field-Methods Training ..................................................................... 15

3.3 Air Monitoring ................................................................................................................... 15

3.3.1 Air-Quality Monitoring Equipment ........................................................................... 15

3.3.2 Air Quality: Exposure Criteria and Actions .............................................................. 16

3.4 Personal Protective Equipment .......................................................................................... 17

3.5 Health Monitoring: Exposure and Heat Stress ................................................................... 19

3.6 Points of Contact ................................................................................................................ 20

3.6.1 Incident Command Operations, Safety Officers, and Other Resources .................... 20

3.6.2 Waste Disposal and Other Environmental Issues ...................................................... 21

3.6.3 Watercraft Decontamination and Vessels of Opportunity ........................................ 21

3.6.4 Accident Reporting .................................................................................................... 21

4.0 Site Setup and Decontamination ............................................................................................. 22

4.1 Work Zones ........................................................................................................................ 22

4.2 Decontamination Procedures .............................................................................................. 26

4.2.1 Cleaning Agents ........................................................................................................ 26

4.2.2 Contaminant Reduction Zone (CRZ): Five-Station Equipment-Decontamination 

Procedure ............................................................................................................................. 27

4.2.3 Post-Decontamination Procedures ............................................................................ 32

4.2.4 Equipment ................................................................................................................. 33

5.0 Multiparameter Sondes: Preparation, Deployment, and Cleaning Procedures ....................... 34

5.1 Sonde Preparation ............................................................................................................... 34

5.2 Methods for Sonde Deployment ......................................................................................... 35
iv

5.2.1 Direct-Dip (Sorbent-Sweep) Method ........................................................................ 35

5.2.2 Plastic Bag Method ................................................................................................... 36

5.2.3 PVC Tube Method ..................................................................................................... 37

5.3 Instrument Decontamination .............................................................................................. 37

5.3.1 Cleaning Procedure ................................................................................................... 37

5.3.2 Decline in Sensor Sensitivity .................................................................................... 38

5.4 Materials and Supplies for Sonde and Sensors Cleaning and Preparation ......................... 38

6.0 Collection of Field Measurements and Water Samples .......................................................... 40

6.1 Objectives and Method Overview ...................................................................................... 40

6.2 Equipment and Supplies ..................................................................................................... 41

6.3 Sampling Location ............................................................................................................. 44

6.4 Step-By-Step Procedures .................................................................................................... 44

6.4.1 Preparation and Order of Sample Collection ............................................................ 46

6.4.2 Peristaltic Pump Method ........................................................................................... 47

6.4.3 Direct-Dip Method .................................................................................................... 51

6.5 Quality Control for Water Samples .................................................................................... 55

6.5.1 Blank Samples ........................................................................................................... 56

6.5.2 Replicate Samples and Matrix Spikes ....................................................................... 58

6.6 Sample Handling and Storage ............................................................................................ 59

6.7 Addendum: Disposable-Bailer Sampling Method ............................................................. 60

7.0 Sediment Samples ................................................................................................................... 63

7.1 Objectives and Method Overview and Preparations .......................................................... 63

7.2 Equipment and Supplies ..................................................................................................... 65

7.3 Site Process and Order of Sample Collection .................................................................... 68

7.3.1 Initial Site Process ..................................................................................................... 68

7.3.2 Order of Sample Collection ....................................................................................... 69

7.4 Step-By-Step Procedures .................................................................................................... 71

7.4.1 Tar-Ball Sample Collection ....................................................................................... 71

7.4.2 Benthic Invertebrate Sample Collection .................................................................... 71

7.4.3 Bulk Sample Collection ............................................................................................. 72

7.4.4 Wrap-Up Procedures ................................................................................................. 75

7.5 Collection of Quality-Control Samples .............................................................................. 75

7.5.1 Equipment Blanks ..................................................................................................... 75

7.5.2 Replicate Samples ..................................................................................................... 77

8.0 Chain of Custody and Documentation Requirements: Labeling, Packaging, and Shipping .. 79

8.1 Method Summary ............................................................................................................... 79

8.2 Field Procedures ................................................................................................................. 79

8.2.1 Field Logbooks and Other Documentation ............................................................... 79

8.2.2 Labeling Sample Containers ..................................................................................... 80

8.2.3 Transfer of Custody and Sample Shipment ............................................................... 82
v 

9.0 Quality Assurance and Quality Control for Field Sampling ................................................... 86

9.1 Quality-Assurance Requirements ....................................................................................... 86

9.2 Summary of Quality-Control Sampling for the USGS Response to the 

Deepwater Horizon Oil Spill .............................................................................................. 87

9.2.1 Frequency and Distribution ....................................................................................... 88

9.2.2 Quality-Control Sample Types .................................................................................. 88

9.3 Definitions and Description of Typical Quality-Control Sample Types ............................ 89

9.3.1 Field Replicates ......................................................................................................... 89

9.3.2 Matrix Spikes ............................................................................................................ 90

9.3.3 Field Blanks ............................................................................................................... 90

9.3.4 Equipment Blanks ..................................................................................................... 91

9.3.5 Source-Solution, Temperature, and Trip Blanks ....................................................... 91

10.0 Selected References ............................................................................................................. 92

11.0 Acronyms, Abbreviations, and Chemical Symbols ............................................................. 98

Appendices

Appendix A. Collection of Baseline Samples in Response to the Deepwater Horizon Oil 

Spill and Location of Pre- and Post-Landfall Sampling Sites ............................................. 102

Appendix B. Field Supplies Recommended for the October 2010 Oil-Spill Sampling. ........ 118

Appendix C. Research Methods ............................................................................................. 122

Appendix D. Post-Landfall Shipping Requirements for Water and Sediment Samples......... 130

Appendix E. Health and Safety .............................................................................................. 139

Appendix F. Examples of a Field Form and Analytical Services Request and Chain 

of Custody Forms Specific to USGS Sampling in Response to the Deepwater 

Horizon Oil Spill ................................................................................................................. 158

Appendix G. Manufacturer Guidance for Use of Multiparameter Sondes in 

Oil-Contaminated Waters .................................................................................................... 168
vi 

Figures

 1. Map showing USGS sites sampled in response to the Deepwater Horizon oil spill, Gulf 

of Mexico, 2010 ............................................................................................................... 2 

 2. Photographs showing Louisiana coastal marshes ............................................................ 5 

 3. Flowchart showing preparations for post-landfall sampling, Gulf of Mexico, 2010..... 10 

 4. Flowchart showing site setup for sampling and equipment decontamination. .............. 24 

 5. Photographs showing the Exclusion Zone delineated by yellow police tape ................ 25 

 6. Photograph showing the decontamination of waders at Station 1 in the 

Contamination Reduction Zone. .................................................................................... 30 

 7. Flowchart showing water-column sampling, Gulf of Mexico Deepwater Horizon oil 

spill, 2010 ....................................................................................................................... 45 

 8. Flowchart showing sediment sampling, Gulf of Mexico Deepwater Horizon oil spill, 

2010................................................................................................................................ 70 

 9. Example of a sample label. ............................................................................................ 81 

 10. Example of a custody seal.............................................................................................. 84 

Tables 

 1. Containers and preservatives specific to water-column sampling. ................................ 42 

 2. General supplies for water-column sampling. ............................................................... 43 

 3. Stabilization criteria for field measurements. ................................................................ 46 

 4. Containers and preservatives specific to sediment collection. ....................................... 66 

 5. Supplies for sediment sampling. .................................................................................... 67 
vii 

Conversion Factors 

Both U.S. customary English (inch/pound) and SI (metric) units of measurement have been used in this report. 

The utility of this report led to the decision to allow mixed units in the text and tables. USGS field personnel 

purchased much of the specialty equipment needed from sources using English units exclusively. In general, 

however, metric units are used to determine sample volume and the volume of chemical preservatives.

Inch/Pound to SI

Multiply By To obtain

Length

inch (in.) 2.54 centimeter (cm)

inch (in.) 25.4 millimeter (mm)

foot (ft) 0.3048 meter (m)

Volume

ounce, fluid (oz) 0.02957 liter (L) 

gallon (gal) 3.785 liter (L) 

barrel (bbl) 42.0 gallon (gal)

Temperature in degrees Celsius (°C) may be converted to degrees Fahrenheit (°F) as follows:

°F=(1.8×°C)+32

Temperature in degrees Fahrenheit (°F) may be converted to degrees Celsius (°C) as follows:

°C=(°F-32)/1.8

SI to Inch/Pound

Multiply By To obtain

Length

micrometer (μm) 3.937 x 10-5 inch (in.)

centimeter (cm) 0.3937 inch (in.)

millimeter (mm) 0.03937 inch (in.)

meter (m) 3.281 foot

liter (L) 33.82 ounce, fluid (oz)

liter (L) 0.2642 gallon (gal)

mlliliter (mL) 0.0338 ounce, fluid (oz)

Area

2 square meter (m ) 0.0002471 acre

Mass

gram (g) 0.03527 ounce, avoirdupois (oz)

kilogram (kg) 2.205 pound avoirdupois (lb)

Specific conductance is given in microsiemens per centimeter at 25 degrees Celsius (μS/cm).
viii

Acknowledgments

The authors wish to acknowledge the efforts of those whose contributions enhanced the 

quality of this report. 

Technical Review

The expertise and recommendations of the following colleague reviewers resulted in 

important improvements to this protocol: Kristen Keteles, U.S. Environmental Protection 

Agency, Region 8; Gunnar Lauenstein, National Oceanic and Atmospheric Administration; 

and C.R. Demas and C.J. Oblinger, U.S. Geological Survey. 

Technical Development

The cooperation and collaboration offered by the staff of the following USGS Water Science 

Centers were indispensible in developing a usable sampling protocol: Alabama, Florida, 

Georgia, Louisiana, Mississippi, and Texas. In particular, we wish to thank M.P. Berndt, 

D.K. Demcheck, A.C. Gill, G.R. Kish, M.J. Lee, M.A. Manning, S.V. Mize, and M.S. 

Runner. The leadership provided by D.N. Myers, Chief, and T.L. Schertz, Assistant Chief, 

Office of Water Quality, and C.R. Demas, Director, Louisiana Water Science Center, is 

gratefully acknowledged. 

Instructions and guidance for preparing samples for laboratory analyses and for maintaining 

sample integrity were developed from information provided by the following USGS research 

scientists: G.R. Aiken, J.M. Biedenbach, K.E. Butler, R.S. Carr, A.W. Demopoulos, R.P. 

Eganhouse, K.L. Elrick, E.T. Furlong, J.L. Gray, A.J. Horowitz, J.T. Lisle, J.W. McCoy, and 

R.J. Rosenbauer. Outstanding support in the execution of this project was provided by G.L. 

Cottrell, P.A. Alex, W.D. Lanier, and M.E. Marshall of the USGS National Water Quality 

Laboratory; E.F. Tillman, chemist with the USGS Hydrologic Instrumentation Facility; and 

Martin Edwards of the TestAmerica Laboratory in Pensacola, Fla. The authors thank the 

following companies for the assistance and expertise of their technical staff: AET 

Environmental, TEC, Inc., In-Situ Inc., and YSI. 

Procedures and regulations regarding the health and safety of field personnel engaged in the 

environmental sampling for which this protocol was developed were provided by U.S. 

Geological Survey (USGS) staff A.E. Zepeda (Bureau Industrial Hygienist), G.L. Hill 

(Bureau Watercraft Safety Program Manager), and Beth Demith (Regional Industrial 

Hygienist); and by D.A. O’Connell, AET Environmental. 

Editorial, Graphics, Layout, and Bureau Approval 

USGS staff members instrumental in supporting the publication of this report were I.M. 

Collies, S.C. Cooper, and C.Y. Knutson. 
1 

U.S. Geological Survey Protocol for Sample Collection in 

Response to the Deepwater Horizon Oil Spill, Gulf of 

Mexico, 2010 

Sampling Methods for Water, Sediment, Benthic Invertebrates, and 

Microorganisms in Coastal Environments

By Franceska D. Wilde and Stanley C. Skrobialowski

1.0 Development of the Post-Landfall Sampling Protocol

In response to the potential for environmental damage to the Gulf of Mexico from a massive 

release of oil caused by failure of the Macondo-1 well and explosion of the Deepwater Horizon 

oil rig, U.S. Geological Survey (USGS) scientists collected environmental data at sites along the 

Gulf coast from Florida to Texas (fig. 1), both before (pre-landfall) and after (post-landfall) oil 

reached shore. The pre-landfall water and sediment samples and relevant site data were collected 

in accordance with official USGS protocols, as directed by a heretofore unpublished sampling 

plan (Appendix A-1) and as prescribed for routine sample collection in the USGS National Field 

Manual for the Collection of Water-Quality Data, also referred to as the National Field Manual

or NFM (U.S. Geological Survey, variously paged, available online only at 

http://pubs.water.usgs.gov/twri9A). All members of field teams engaged in pre- and post-landfall 

sampling were to have completed formal training and be experienced in the sampling methods 

established in the NFM. 

While the National Field Manual provided the field teams with the methods and procedures 

needed for the pre-landfall field effort, it lacked the information needed to meet the regulatory, 

health-and-safety, and logistical requirements for conducting field activities at heavily oilimpacted and potentially hazardous sites. As a result, the USGS developed this U.S. Geological 

Survey Protocol for Sample Collection in Response to the Deepwater Horizon Oil Spill, Gulf of 

Mexico, 2010 to augment the protocols, methods, and procedures stipulated in the National Field 

Manual in order to provide post-landfall field teams with the explicit requirements and guidance 

needed for sampling potentially hazardous substances under potentially hazardous conditions. 

“Post-landfall” refers to conditions along the Gulf of Mexico coastline following the shoreline 

arrival of oil from the Deepwater Horizon well failure and ocean-bottom oil release. Site 

deployment and sample collection under these conditions necessitated modifications to standard 

USGS sampling and analysis procedures. 

The first version of the post-landfall sampling protocol was published in September 2010 

(http://pubs.usgs.gov/of/2010/1191/) to provide authorities responsible for the oversight of oilresponse activities, other agencies and organizations collecting post-spill data in the Gulf of 

Mexico, and USGS field teams with USGS sample-collection plans at Gulf Coast sites at which 

oil was expected to encroach. The protocols subsequently were field tested and revised to 
2 

account for changed and changing conditions on the ground. This report incorporates 

modifications to the protocol since it was first published, and also includes the pre-landfall 

sampling plan (Appendix A–1), a list of the laboratory analyses performed for this project 

(Appendix A–2), a list of the sites and dates sampled (Appendix A–3), and location maps of the 

pre- and post-landfall sites sampled (Appendix A–4). 

Figure 1. Map showing USGS sites sampled in response to the Deepwater Horizon oil spill, Gulf of Mexico, 2010.
3 

1.1 Background 

On April 20, 2010, the Deepwater Horizon oil rig exploded, resulting in release of crude oil into 

the northern Gulf of Mexico from the ruptured British Petroleum (BP) Macondo-1 (BP M-1) 

well. By July 15, 2010, an estimated 4.4 million barrels (approximately 185 million gallons)1 of 

oil had entered Gulf waters (Crone and Tolstoy, 2010), posing a potential threat to the viability 

of sensitive habitats and other critical and unique environmental resources along the Gulf of 

Mexico shoreline (fig. 2).

The initial response of the USGS was to mobilize as rapidly as possible to collect samples and 

data before landfall of the oil in order to establish a baseline chemical and biological profile 

against which to understand any post-landfall effects on, or changes to, Gulf of Mexico coastal 

environments. USGS Water Science Centers in Texas, Louisiana, Mississippi, Alabama, and 

Florida coordinated efforts to sample water and sediments at 70 sites from beaches, barrier 

islands, and coastal wetlands that could suffer severe environmental damage as a result of oil 

from the spill coming ashore. Pre-landfall data collection occurred from May 7 through July 7, 

2010. 

Post-landfall collection of coastal sediments and nearshore water by the USGS was initiated in 

October 2010, following a request by the U.S. Coast Guard (USCG) to assess the existence of 

“actionable” levels of Deepwater Horizon-related oil-spill contamination after extensive cleanup 

efforts of coastal areas by BP. Sampling was carried out at 48 of the original 70 sampling sites 

that were considered at highest risk for oil contamination and environmental degradation. In 

addition, one “oiled” wetland site was sampled on August 23, 2010, as part of a separate project 

to coordinate collection of ground data at Bay Jimmy, La., with data collected during an AVIRIS 

(Airborne Visible/Infrared Imaging Spectrometer) overflight. 

U.S. Geological Survey field teams collected post-landfall samples and site data by following the 

protocols and procedures laid out in this report in addition to those articulated in the USGS 

National Field Manual (U.S. Geological Survey, variously paged). Appendix A in this report has 

been expanded to include the guidelines used for the pre-landfall sampling effort in addition to a 

list and map locations of the 70 pre-landfall and 49 post-landfall sampling sites.

1.2 Objective and Approach

The objective of the October 2010 post-landfall sampling effort was to document environmental 

indicators at 49 of the 70 sites previously sampled; that is, at the subset of sites deemed most 

vulnerable to oil contamination. Comparisons of pre- and post-landfall sample analyses are used 

to document the presence of oil related to the Deepwater Horizon incident and, by use of oil 

fingerprinting analysis, to distinguish it from historic (pre-Deepwater Horizon) oil. Samples also 

were analyzed for concentrations of polycyclic aromatic hydrocarbons (PAHs), oil and grease, 

metals and other trace and major elements, nutrients, volatile and semi-volatile organic 

compounds, total petroleum-range and diesel-range hydrocarbons, dissolved organic carbon, 

 

1 Both U.S. customary English (inch/pound) and SI (metric) units of measurement have been used in this report. The 

utility of this report led to the decision to allow mixed units in the text and tables. USGS field personnel purchased 

much of the specialty equipment needed from sources using English units exclusively. In general, however, metric 

units are used to determine sample volume and the volume of chemical preservatives.
4 

residue of the Corexit surfactant used to disperse the oil released to the Gulf of Mexico, and to 

identify the status of benthic invertebrate populations, characterize oil-digesting bacterial 

populations, and examine the toxicity of pore waters extracted from sediment samples (Appendix 

A-2). Profiles of the research scientists and laboratories used for this work can be found in 

Appendix C. 

1.3 Purpose and Scope

This report was intended originally as an addendum to the National Field Manual, to provide 

USGS field teams with the general information and protocols needed to meet the requirements 

associated with working in an oil-impacted environment that poses a potential hazard to human 

and environmental health. The urgency of the rapidly mobilized response to the oil spill dictated, 

however, that these protocols incorporate a level of detail specific to that response. This report, 

while describing protocols and procedures that are relevant to oil-spill environmental 

investigations in general, has been focused to address the practical and immediate needs of 

USGS field teams charged with collecting the data needed to underpin scientific investigations in 

the northern Gulf of Mexico related to the Deepwater Horizon oil spill. The reader is advised, 

therefore, that any names, e-mail addresses, phone numbers, and other contact information that 

are included in this report were relevant to the October 2010 operation only and have since been 

discontinued or superseded. The information provided in this report was designed to facilitate 

and document field preparations and address the necessary data-collection requirements and 

guidance specific to this sampling effort. 
5 

A 

B 

Figure 2. Photographs showing (A) a pristine Louisiana coastal marsh and (B) oil encroaching on a Louisiana coastal marsh. 

Photographs by Dennis Demcheck, U.S. Geological Survey.
6 

2.0 Preparations for Sampling at Oil-Contaminated Sites

Multimedia sampling associated with this response to the Deepwater Horizon oil spill involves 

the collection of surface-water, sediment, benthic invertebrate, and microorganism data at 

potentially hazardous sites along the northern Gulf of Mexico coastline. The preparations 

required to accomplish the proposed field work follow, as applicable, from the procedures 

established in chapters 1 through 7 of the National Field Manual for the Collection of WaterQuality Data (see U.S. Geological Survey, variously dated). The National Field Manual

currently does not, however, provide the detailed guidance needed for sample and data collection 

at field sites that are considered by regulatory agencies to include oil-contaminated “exclusion

zones” or “hot zones.” This report, therefore, augments the standard protocols established in the 

NFM to ensure the legal and scientific defensibility of data collection and associated field 

activities at sites considered to include exclusion zones in Gulf of Mexico coastal areas. Before 

beginning field activities, therefore, it is necessary for field personnel to be familiar with the 

procedures, requirements, and implementation of NFM protocols in addition to those laid out in 

this report. For this project, a three-person field team generally is required for collection of 

water and sediment samples; site-related field operations may dictate additional field 

personnel. A synopsis of the equipment and preparations needed to carry out field activities for 

this project are provided in this section and are summarized in Appendix B. 

2.1 Communication with Incident Command 

USGS personnel are to contact the Incident Command (IC) or Unified Command (UC), as 

applicable, two or more days in advance of deployment to the field site to obtain the “Daily 

Operational and Safety Situational Report” (the “shift” or operations plan) for their sampling 

area or sector. The IC/UC may request a description of planned field activities and typically 

requires personnel to carry an IC-generated identification pass in addition to official USGS 

identification.

2.2 Training and Safety

All personnel involved in Deepwater Horizon Post-Landfall field activities require 4 hours of 

training provided by British Petroleum (BP) in addition to formal Hazardous Waste Operations 

(HazWOper) training. HazWOper training consists either of the 40-hour or 24-hour training or 

the 8-hour HazWOper refresher (for those having had the 40-hour training over 1 year ago), as 

detailed in Section 3 of this protocol. 

Field personnel also are required to have completed the USGS Water-Quality Field Methods 

course (QW1028) or the Field Methods Refresher course (QW3190) within the last 5 years, and 

the Motorboat Operator Certification Course (MOCC) for those operating motorboats to access 

sampling sites.

The safety procedures outlined in this protocol are required when entering oilcontaminated areas and are described in detail in Section 3. These procedures mandate 

monitoring and mitigating the effect of exposure to toxic and combustible compounds associated 

with the oil release and use of Level D personal protective equipment, including organic vapor 

analyzers (photoionization detectors), as appropriate to site conditions and required by 
7 

HazWOper training. Site-specific safety precautions must be identified and addressed adequately 

in a site-specific Health and Safety Plan (HASP); the provisons in the HASP must be 

acknowledged and implemented by all members of the field team. 

2.3 Equipment and Supplies

Field personnel must allow sufficient time to order and obtain, test, quality assure, and 

familiarize themselves with the equipment and supplies required for this water- and sedimentsampling operation. A list of recommended equipment and supplies can be found in Appendix B, 

with additional information given in each section of this report (for example, Section 5, for field 

measurement instruments, and Section 6, for water sampling). 

• Use of a photoionization detector (PID) is required when working in areas contaminated 

by petroleum products (see Section 3.0). 

• A Global Positioning System (GPS) instrument is used by each team to document and 

verify site and sampling locations. In addition, documentation of site and sampling 

location, features, and conditions requires use of a digital camera, maps, and a bound log 

book (see Section 8.2.1). 

When ordering or assembling articles for the field effort, it is important to include backup, spare, 

and extra equipment. Spare equipment/supplies includes all that might be needed for sample 

collection and processing, such as sample containers and labels; capsule filters; backup meters, 

calibration solutions, and batteries; Teflon core tubes, scoops and bucket liners; an assortment of 

gloves and glove sizes; field forms, including those for chain-of-custody; decontamination and 

exclusion zone materials and supplies. It is necessary, for example, to order a sufficient number 

of sample containers so as to have at least one spare set onsite plus a sufficient number of 

containers for collection of quality-control samples. 

• Sample containers and chemical preservatives are obtained from the TestAmerica 

Laboratory, Inc. (TAL) in Pensacola, Fla., for samples that will be analyzed at TAL. Some 

sample containers already contain the chemical preservative required for the respective 

analysis and must be handled with caution. 

• Supplies and sample containers for samples to be analyzed at USGS research laboratories 

are obtained through the USGS National Field Supply Service (NFSS) of the National 

Water Quality Laboratory (NWQL). 

• Containers, sample-collection and -processing equipment, articles needed for equipment 

decontamination, and supplies for shipping, record keeping, and documentation that are 

not available from NFSS are obtained on the open market. 

Any equipment that will be in contact with the sample must be pre-cleaned and quality assured 

as prescribed in the USGS water-quality National Field Manual. Equipment blanks must be 

collected to determine if sample-collection and sample-processing equipment could bias 

analytical results (see Sections 6, 7, and 9). It is important that equipment-blank results be 

obtained and assessed before field work begins, to the extent possible, so that any corrective 

action can be taken, if needed. 
8 

2.4 Prepare for Field Deployment

Field teams should allow several days to assemble gear; prepare coolers, labels, and paperwork; 

and make logistical arrangements with Incident Command and the shippers of samples. In many 

cases two vehicles are needed to transport the gear. 

• Create a checklist of all the equipment and supplies to be transported. 

• Create and review a workplan that includes the types of environmental and quality-control 

samples to be collected.

• Prepare a logbook, paperwork, and labels ahead of time to the extent possible. 

• Label coolers with the type of samples they will contain. Coolers used for transport or 

storage of food, water, decontamination supplies, and so on, also must be separate and 

clearly labeled.

• Prepare and check maps for emergency routes and facilities. 

• Make a copy of this protocol document to keep in the field; print out Appendix D 

separately for quick reference.

• Be familiar with and test the operation of the GPS, PID, camera, and other such equipment 

and instruments. 

• Some sampling locations will be accessed by boat; therefore, USCG clearance as well as 

all training, certifications, and equipment necessary to conduct these activities safely and 

efficiently must be available and in order. Appropriate arrangements should be in place for 

and decontamination of the vessel (Section 4.0). 

2.5 Initial Onsite Preparations

Upon arrival at the field site, the field team must: 

1. Evaluate and record field conditions with respect to provisions of the site-specific Health 

and Safety Plan (see Section 3.0); 

2. Define the exclusion zone (EZ), contamination reduction zone (CRZ), support zone (SZ), 

and contamination reduction corridor (CRC) (described in Section 4.0) for sampling and 

equipment decontamination before sample collection can begin; 

3. Evaluate and document the nature and extent of apparent oil-spill-related contamination 

at the time of site visits; 

4. Refer to these protocols and previous sampling training and experience to select and 

implement the appropriate environmental and quality-control sampling and datacollection methods and procedures (Sections 4, 5, 6, 7, 8, and 9); 

5. Follow explicitly all chain-of-custody (CoC) and documentation requirements (Section 

8). All samples collected for this project must be collected and shipped in accordance 

with CoC procedures; and

6. Maintain a logbook in which the date/time, place, personnel, visitors, site conditions, and 

procedures and methods used must be recorded (Section 8). 
9 

The flowchart in figure 3 shows the major considerations and actions needed before deploying to 

the field site. Similar flowcharts are included in Section 4 for equipment decontamination 

(fig. 4), in Section 6 for water sampling (fig. 7), and in Section 7 for sediment sampling (fig. 8). 

Appendix D includes two very useful tables, one for water sampling and one for sediment 

(solids) sampling, that list container requirements for each analysis, summarize how the samples 

should be preserved and shipped, and list laboratory contacts and addresses. Printing copies of 

the flowcharts and the Appendix D tables is recommended to serve as quick reference guides for 

field work. 
10 

Figure 3. Flowchart showing preparations for post-landfall sampling, Gulf of Mexico, 2010.
11 

3.0 Safety in Field Activities

Large-scale petroleum releases can result in various scenarios for human exposure. The hazards 

of exposure should not be underestimated when planning to work in affected areas. The Health 

and Safety Plan (HASP) and other safety procedures and precautions outlined in this section of 

the protocol are required for USGS personnel entering oil-contaminated areas. The protocol 

includes procedures for safe work practices, working in exclusion zones, personal protective 

equipment (PPE), training, and identification of contacts to assist with response to onsite 

conditions and emergencies. Much of the information covered in this section, as well as 

examples of HASP documents, are included in greater detail in Appendix E. In brief, the safety 

requirements described in this section will mandate:

• Development of site-specific HASPs and Job Hazard Analyses (JHA). 

• HazWOper and British Petroleum (BP) training specific to the Gulf of Mexico: Plan on 

24 or 40 hours of HazWOper training, plus an additional 4 hours of BP training 

(see explanation in 3.2 below). (In addition, OSHA generally requires medical 

monitoring and CPR/First-Aid Certification training; this is not covered in this 

document.) 

• Two-week Water-Quality Field Class training. 

• Motorboat-Operator training and certification for personnel piloting water vessels.

• Air-quality monitoring. Photoionization detection (PID) that exceeds the 20 parts per 

million by volume (ppmv) action level for total volatile organic compounds will result in 

evacuation of the field site.2

• PPE including Tyvek apparel, PFDs, latex overboots or rubberized waders, eye protection, 

rubberized elbow-length gloves and nitrile hand gloves, used as described in the protocols 

for sample collection and handling. 

• Strict adherence to HazWOper training and preventing heat stress is required, including 

mandatory rest periods every 15 to 30 minutes. DO NOT NEGLECT THIS 

MANDATE.

Changing field conditions may require modifications to these protocols as they apply to Gulf of 

Mexico oil-spill sampling. Protocol changes will be communicated to field teams and 

supervisors electronically, as needed. Familiarization with the guidance provided in this section 

does not replace the requirement to read and understand the HASP (Appendix E). 

 

2 The U.S. Geological Survey or Department of the Interior industrial hygienist determines if and when PID use can 

be halted. Use of respirators and monitoring air quality for exposure to benzene are not included in this protocol as 

they are not relevant to the field conditions planned for USGS shoreline sampling for the 2010 Deepwater Horizon 

project. 
12 

TAKE NOTE! Field personnel are required to stop work and rest at the first sign of heat 

discomfort; do not overextend your limits. It is the responsibility of every team member to 

monitor each other for signs of overheating or other evidence of deteriorating health.

3.1 Health and Safety Plans

The Occupational Safety and Health Administration (OSHA) requires the development of sitespecific Health and Safety Plans (HASPs) that must be given in hard copy to each employee 

performing oil-response or site-cleanup activities. The field-team leader or supervisor has the 

responsibility to ensure that the safety protocols and their expectations are understood by each 

member of their field team. 

The USGS has produced a template that can serve as the basis for developing a site-specific 

HASP for oil-contaminated areas. Some of the information required to populate this template 

may be included in the Daily Operational and Safety Situational Report (Shift Plan) described 

below. The Incident Command contact or USGS regional safety/industrial-hygiene staff can be 

called on to provide additional assistance regarding requirements for the HASP. 

USGS HASP requirements for response to the Gulf of Mexico (GOM) Deepwater Horizon 

(DWH) oil spill are fulfilled by assembling a USGS DWH GOM HASP package, which should 

be kept on hand when deploying to the field site. This package includes the following 

documents, some of which are included in Appendix E and that USGS personnel can download 

by opening “HASP Package” found at https://my.usgs.gov/OWQ_Deep_OilWiki/3

: 

1. Agency HASPs. A HASP provided by the Incident Command (IC) or agency under 

whose jurisdiction the work will be conducted should be appended to the site-specific 

HASP, described above. In the case of this project, the HASP provided by the U.S. Fish 

and Wildlife Service (FWS) will suffice, unless directed otherwise. The links for USCG 

and FWS plans given below are specific to the current oil release in the Gulf of Mexico

and may become inactive at the close of investigations related to this incident. 

a. U.S. Coast Guard (http://www.uscg.mil/forms/ics/ICS_208_CG.pdf) 

b. Available to USGS personnel from FWS: 

http://internal.usgs.gov/ops/safetynet/FWS%20WIldlife%20Branch%20HASP%20(M

C%20252%20Oil%20Spill).pdf.

2. The Daily Operational and Safety Situational Report (the “Shift” or Operations 

Plan). The Shift Plan, which may cover a 24- or 48-hour time period or longer, is to be 

obtained in advance from the designated IC safety or industrial hygiene staff for the 

day(s) of field deployment. Contact information for this project is described in Section

3.6; however, the responsible parties shift in and out of their respective positions 

frequently, requiring field teams to consult the latest Shift Plan. 

 

3 https://my.usgs.gov/OWQ_Deep_OilWiki/wiki/Main; non-USGS parties may request access by contacting 

fwilde@usgs.gov or sski@usgs.gov and providing the rationale for their request.
13 

a. To avoid delay of field work, arrangements should be made within two or more days 

in advance to receive the Shift Plan via e-mail for the time period of planned field 

deployment. 

b. The field-team leader or representative also should request information about the 

accessibility to 911 or other emergency contacts at the site(s) to be visited. 

c. Field personnel must be briefed on the health and safety information given in the 

Shift Plan before commencing with field work; this includes, for example, weather 

conditions, heat-index values, official emergency evacuation plans, and current 

emergency contacts. 

d. The Shift Plan fulfills the requirement that the HASP include the specific information 

covering health, safety, and hazardous conditions that pertain to USGS sampling sites

on the days of sampling and to keep an up-to-date list of operational and emergency 

contacts on hand. 

3. Evacuation Plan. Evacuation plans may or may not be included in the Shift Plan. 

Evacuation plans are specific to and provided by the Huoma, La., or Mobile, Ala.,

Incident Commands for this project. The field team should request the latest evacuation 

plan when requesting the Shift Plan and include it in their HASP package. 

4. Site-specific job and work-site hazards (Job Hazard Analysis or JHA). Those hazards 

that have not been included in the HASP or Daily Report should be added to the JHA, as 

is illustrated in the example JHA in Appendix E. Any other hazards that are identified 

onsite also should be recorded on the JHA form upon arrival onsite, along with the 

actions to be taken to eliminate or reduce the hazard(s) noted. 

a. JHAs for the handling of dry ice, chemical preservatives such as hydrochloric acid and 

formalin (see NFM 9.6), and other types of equipment can be accessed at the following 

URL, and should be downloaded and added to the HASP package 

http://1stop.usgs.gov/safety/topic/jha/index.html. 

b. Wildlife hazards, such as snakes, alligators, and ticks and mosquitoes need to be 

identified and plans in place for a safe and appropriate response—refer to chapter 9 of 

the National Field Manual at 

http://water.usgs.gov/owq/FieldManual/Chap9/content.html (U.S. Geological Survey, 

variously paged). 

5. Site setup for sampling hazardous materials. Standard procedures for avoiding contact 

with and removal of hazardous materials, including setting up exclusion and 

contamination reduction zones, normally are included in a HASP developed for exposure 

to environmental release of petroleum products, as detailed in Section 4.0. 
14 

3.2 Training 

The training specified below is a prerequisite for USGS personnel whose duties will require field 

work in oil-contaminated areas, operation of a motorboat, and who will be engaged in onsite data 

and sample collection. 

3.2.1 HazWOper and British Petroleum Training 

USGS personnel entering exclusion or “hot” zones (see Section 4) to collect samples are required 

to complete HazWOper training, plus an additional 4 hours of training from BP, as described 

below. 

The Incident Command requirement stipulates a minimum of 24 hours of HazWOper training for 

nonsupervisory onsite personnel and 40 hours of training for “supervisory” personnel (defined as 

one who has authority, control, and oversight of the activities performed at the site). The 40-hour 

training course is recommended for all USGS field personnel, as any member of a USGS field 

team may be asked to take on supervisory duties. 

• If no one has been given onsite responsibility, or when an onsite supervisor is not present, 

the individual who is supervising field activities from an offsite location is required to 

have completed the 40-hour HazWOper training. 

• The 8-hour refresher course for HazWOper training is required for personnel whose 

HazWOper training is not current. Initial and refresher training certification expires 12 

months from the completion of the last training.

• For this project, USGS employees can take HazWOper training online through the FWS 

vendor at no cost. Select the course below to register, then select “U.S. Fish and Wildlife” 

as the company name. Leave the bottom (payment) portion blank, as billing arrangements 

have been made. After clicking to submit your registration, the course opens immediately. 

Your place is saved automatically if you leave the training session before finishing. 

− 40-hour HazWOper training - 

https://www.natlenvtrainers.com/register.html?course=40HazWOper

− 24-hour HazWOper training - 

https://www.natlenvtrainers.com/register.html?course=24HazWOper 

− 8-hour HazWOper Annual Refresher training - 

https://www.natlenvtrainers.com/register.html?course=HazWOper

• Other vendors approved to provide classroom or electronic HazWOper training can be 

found at ERTP Virtual University

(http://www.ertpvu.org/kc/login/login.asp?kc_ident=kc0001). Registration is required to 

access the site. Once logged on, select the external provider from the left side of the screen 

and then select the List of EPA Approved External Providers to locate vendors. 

• In addition to the HazWOper training, all field personnel engaged in this project must take 

the following 4-hour online BP training, regardless of previous or current HazWOper

training (instructions for taking this training are provided in Appendix E): Post Emergency 
15 

Spilled Oil Cleanup (HSEREH004) 

https://www2.virtualtrainingassistant.com/BPPublic/wc.dll?learner~cmenu. 

3.2.2. Motorboat Operation

All USGS personnel who operate a motorized watercraft vessel less than 26 feet in length for 

Gulf coast sampling are required to complete the Department of the Interior Motorboat Operator 

Certification Course (MOCC). This course involves "hands-on" watercraft activities, including 

watercraft handling and maneuvering, docking, emergency procedures, fire suppression, and 

trailering exercises, as well as classroom instruction. MOCC Certification is valid for 5 years and 

recertification is available either online or in combination with a MOCC Instructor. 

3.2.3 Water-Quality Field-Methods Training

QW1028, the 2-week course on “Groundwater and Surface-Water Water-Quality Field 

Methods,” contains protocols and guidance on safety when sampling under a variety of 

environmental conditions and using various chemical agents. This course is based on the USGS 

National Field Manual (U.S. Geological Survey, variously paged), which also contains a chapter 

on “Safety in Field Activities” (Chapter A9). All USGS personnel engaged in on-site sampling 

and data collection for this project should have completed the 2-week classroom and hands-on 

course or its refresher course within the past 5 years and have experience implementing the 

protocols and procedures provided within each chapter of the water-quality National Field 

Manual. At a minimum, the field team leader and one other team member must be current 

in this water-quality field-methods training.

3.3 Air Monitoring 

Air monitoring is required to determine if a given area is receiving volatilized petroleum 

compounds at a level that may present a hazard to human health. The Department of the Interior 

(DOI) has set a limit on respiratory exposure to total VOC (volatile organic compounds) of 

20 ppmv.4 The U.S. Environmental Protection Agency (USEPA) maintains a database of airmonitoring results at http://www.epa.gov/bpspill/air.html. 

3.3.1 Air-Quality Monitoring Equipment 

In general, a combination meter that includes a photoionization detector (PID) and a lower 

explosive limit (LEL)/upper explosive limit (UEL) meter is recommended when exposure to 

petroleum-based products is anticipated. Depending on the situation, monitoring of benzene 

concentrations might need to be added to the HASP.5 For the Gulf of Mexico shoreline work, a 

 

4 16 June 2010 e-mail from Robert J. Garbe, Office of Occupational Health and Safety, U.S. Department of the 

Interior: “A 5 ppm cut point for the PID is too low to minimize false positive readings. Recommend that a 20 ppm 

initial cut point be used. Also recommend any excursion above this level be reported to the USGS Safety Office for 

input and guidance prior to reentering the area.” 5 OSHA (Occupational Safety and Health Administration) guidance stipulates a permissible exposure limit (PEL) of 

1 ppm and a short-term exposure limit (STEL) of 5 ppm for benzene. The STEL is based on a 15-minute excursion 

average, while the PEL is based on an 8-hour average; that is, over an 8-hour excursion the average benzene 

concentration is not to exceed 1 ppm.
16 

single-function PID should be used to monitor for organic vapors in the ambient and breathing 

zone during sampling activities. An LEL/UEL meter is recommended if there is a source of 

ignition (such as a boat engine) in the area. 

All air-quality monitoring equipment shall be field-calibrated daily before use and in accordance 

with the manufacturer’s instructions. Anyone calibrating or using the air-monitoring equipment 

should be trained and familiar with exposure-monitoring instrumentation. The time of calibration 

and ambient measurements are to be recorded in the field logbook and the data are to be recorded 

on the field form (Appendix F). 

3.3.2 Air Quality: Exposure Criteria and Actions

Personnel are to evacuate the immediate area if the total VOC concentration indicated by 

the PID reaches 20 parts per million by volume (ppmv). It is necessary to report exceedance 

conditions to the USGS or FWS Industrial Hygienist for input and guidance before reentering the 

area (written commun., DOI Office of Occupational Health and Safety, 2010). The USGS 

Industrial Hygienist has authority to advise when PID scans are not or are no longer necessary.6

• To avoid potential inhalation of vapors, personnel should be positioned upwind of free 

product in the water or on land and upwind of field vehicles or other petroleum-containing 

or -burning equipment. If this is not possible the team leader will determine if the health 

and safety of personnel are at risk and if sampling should be aborted. 

• Field personnel must evacuate the site if PID action levels are exceeded. Do not enter or 

reenter the site until concentrations fall below the action limit unless properly fitted 

respirators are at hand and the team leader determines that sample or data collection can 

continue. Personnel for this project, however, will not be placed in any situation requiring 

respirators. 

• Personnel who experience symptoms of exposure while onsite, even if monitored 

concentrations are less than the action limit, are to evacuate the site and to contact the 

Safety Point of Contact for specific guidance (see Section 3.6). 

PID readings should be recorded: 

• Upon initial entry to the area.

• Every 10 to 30 minutes, or as often as practical while in the breathing zone while work is 

in progress, as long as the PID reading does not appear to be increasing and does not 

exceed 20 ppmv. 

• When weather conditions change. 

• When adverse conditions are encountered, such as exposure to fresh crude oil or noticing 

an increase in odors since initial entry. 

• When work begins on another portion of the site (for example, moving from water 

sampling to the collection of sediments and other solid materials).

 

6 By the start of the post-landfall sampling on October 5, 2010, field teams were notified by the USGS Industrial 

Hygienist that PID scans were no longer required at Gulf of Mexico coastal areas.
17 

U.S. Department of the Interior) Industrial Hygienists collect air samples and air-sample data to 

characterize exposures for DOI employees involved in the response activities. USGS Safety and 

Health Industrial Hygienists are using this information to develop safety and health requirements 

and guidelines. At the end of field operations, copies of field forms containing air-monitoring 

results should be sent to the USGS Bureau Industrial Hygienist. Air–monitoring results for the 

Gulf of Mexico can be found under the following URLs: 

• USEPA: http://www.epa.gov/bpspill/air.html

• Current Air Quality along the Gulf Coast: http://gulfcoast.airnowtech.org/

3.4 Personal Protective Equipment

The recommendations in this section regarding personal protective equipment (PPE) have been 

developed from information taken from U.S. Department of Health and Human Services, 

National Institutes of Health, regarding the current crude oil spill, and from DOI and USGS 

Health and Safety officials. To the extent possible, disposable PPE will be used to minimize the 

risk of skin contact with potentially contaminated sediment or water and to minimize extensive 

PPE decontamination procedures. A list of recommended PPE is at the end of this discussion and 

in Appendices B and E.

All personnel working in a near-shore or off-shore environment must wear a properly fitted 

Personal Flotation Device (PFD) as described in USGS Safety Bulletin “Personal Flotation 

Device Selection/Use,” issued 07/22/2010 (Appendix E). Hearing protection is recommended 

when working in the vicinity of boat motors or other loud equipment. Protocols and procedures 

for discarding oil-contaminated clothing and materials are described in Section 4.

• Personnel working in water affected by free product are required to wear modified 

Level D clothing, including: disposable Tyvek coveralls or pants, safety glasses, and 

disposable nitrile gloves (for handing sample containers and chemical preservatives); and 

nondisposable (cleanable) PFDs, rubber waders, and elbow-length rubber gloves. 

• Waders should be worn over Tyvek apparel. If working in conditions where water 

could enter the waders, the top of the wader should be taped to the underlying apparel with 

duct or Chemron tape. If working in shallow water for which waders are not required, 

latex waterproof boots should be worn over waders and taped to Tyvek pants to form a 

seal, as water will leak through Tyvek seams. Waders should be removed and cleaned 

once back on shore. 

• PFDs should be worn over the Tyvek and wader suspenders when working in water 

and should be adequately cleaned or discarded (see Section 4) if soiled by free product or 

other contaminant. 

− Where there is a potential for oil contamination, the Revere Type V Model 280 Work 

Vest (nylon-buckle closure) PFD has been recommended. This PFD should be used 

and modified as follows to meet DOI standards: obtain pre-cut patches of SOLAS 

adhesive-backed reflective tape from the Bureau Watercraft Safety Program Manager 
18 

along with a detailed drawing of where to attach the tape. The Type V Model 280 

PFD can be cleaned of oil using soap and water or alcohol swabs. 

− The standard Type 3 PFD supplied to USGS personnel may be worn where there is 

no potential for oil contamination; however, should the PFD become contaminated 

with oil or oil-related product, the PFD may not be reused and must be disposed of as 

hazardous waste. 

• Take care to prevent skin contact with contaminated water and sediments by wearing hand 

and arm protection (Sections 5, 6 and 7). Elbow-length rubberized gloves are worn over 

layered nitrile gloves. Do not reach into contaminated water to collect samples without 

wearing appropriate gloves. Rubberized gloves can be cleaned as described in Section 4. 

Disposable (nitrile) gloves need to be replaced often and disposed of as described in 

Section 4. 

• Splash shields or safety glasses are worn to protect eyes from splashes during sampling, 

decontamination procedures, or boat travel. 

• Personnel working on land also are required to wear modified Level D clothing. 

• Use latex boots instead of Tyvek boots; Tyvek shreds readily when walking on beach 

sands. 

List of recommended PPE: 

• Calibrated PID, possibly in combination with an explosimeter (LEL/UEL meter) and 

benzene sensor. 

• National Institute of Standards and Technology (NIST) traceable calibration gases and 

regulators for the specific instrumentation. 

• Operator’s Manual for PID/UEL instrumentation. 

• Eye protection (safety glasses, splash shield, goggles, as appropriate). 

• Nitrile gloves. 

• Rubberized gloves, elbow-length or longer. 

• Tyvek pants or coveralls. 

• Latex waterproof overboots (as appropriate). 

• Rubberized (cleanable) hip or chest waders. 

• PFD, Revere Model 280 Type V work vest (available from, for example, WestMarine/Port 

Supply, “Model # 10967776) with nylon-buckle closure. This PFD must be modified to 

conform to the USGS standard for PFD reflectivity (Section 3.3 above). 

• PFD, standard Type 3, as specified in USGS Safety Bulletin 7/22/2010 (Appendix E). 

• Duct or Chemron tape. 

• Insect repellent (noncontaminating) and head nets. 

• Steel-toed shoes/boots (as specifically required by work task). 

• Hard hat (as specifically required by work task). 
19 

3.5 Health Monitoring: Exposure and Heat Stress 

Ingestion of contaminated materials is minimized by good personal hygiene and taking the 

appropriate cautions while handling materials and solutions associated with petrochemical 

contamination and equipment decontamination (that is, by thoroughly washing face and hands 

with soap and water, especially before eating or drinking). 

The Heat Index (HI) is the temperature the body feels when heat and humidity are combined. It 

sometimes is referred to as the "apparent temperature." The HI, given in degrees Fahrenheit (oF), 

is a measure of how hot it feels when relative humidity is added to the actual air temperature. 

The National Oceanic and Atmospheric Administration (NOAA) posts a heat-index calculator at 

http://www.hpc.ncep.noaa.gov/html/heatindex.shtml; the heat index also can be found from the 

National Weather Forecast. HazWOper training and subsequent refresher training should include 

prevention and identification of heat stress-related injuries and illnesses. Field personnel must 

record the Heat Index (HI) in their field notes (this information should be included in the 

Shift (Operational) Plan described in Section 3.1 above). 

The Heat Stress Prevention Program outlines exposure controls to protect employees working in 

hot environments and follows current American Conference of Governmental Industrial 

Hygienists guidelines. These are general guidelines that need to be tailored to provide specific 

guidance for the work site. The Heat Stress Prevention Program is implemented when workarea temperatures rise above 90°F when Level D PPE is worn. Work practices and exposure 

controls are used to reduce the risk of elevating an employee’s core body temperature. These 

work practices and exposure controls, detailed in the HASP package, include the following: 

• Defining and adjusting employee work/rest intervals.

• Monitoring for physiological signs of heat stress. 

• Providing cool liquids at the ratio recommended in the site-specific Shift Plan. 

• Establishing and implementing acclimatization schedules.

TAKE NOTE! Wearing PPE can increase your risk for heat stress, exhaustion, and heat 

stroke when working in hot climates or at elevated levels of temperature and humidity. 

• Stay hydrated and be alert to signs of headaches, dizziness, nausea, cramps, and 

profuse sweating followed by no sweating in yourself and others. 

• Do not push yourself. Switch sampling duty among team members every 30 minutes 

or less.
20 

3.6 Points of Contact

Points of contact refer to those offices or individuals having responsibility over a specific 

function related to the oil-spill response. These personnel often rotate in and out of a given 

position along with their phone number, making it necessary for field personnel to obtain up-todate contact information for the period of field work. This information is provided in the Shift 

(Operational) Plan. 

 For this project, the team leader obtains the Shift (or “Ops”) Plan from the Houma (Texas and 

Louisiana Water Science Centers) or Mobile (Alabama, Mississippi, and Florida Water Science 

Centers) Unified Command Sector Safety Officer ahead of field deployment (Section 3.1). The 

information below shows the office to be contacted for a given function or need and, if available, 

provides contact information that is persistent and therefore, in general, not subject to change. 

For this project, the IC/UC or FWS Safety Officer on duty is the primary coordinating 

contact.

3.6.1 Incident Command Operations, Safety Officers, and Other Resources 

USGS personnel should notify the local Incident Command (IC) Center about the location and 

the type of work being done. The IC staff advises on areas that are off limits, or if IC 

authorization is required to enter certain areas. USGS personnel can obtain current guidance on 

safety and health issues, such as known hazardous conditions, from their local and Regional 

Safety staff if primary points of contact are not available.

Incident Command and Safety Officers

• Houma, La., Incident Command - 1697 Highway 311, Houma LA 70395, Main 985-493-

7600; Operations 985-493-3343; mc252decon@gmail.com 

• Mobile, Ala., Incident Command - One South Water Street Mobile AL 36602, 251-442-

1938. 

• Houma Sector, Wildlife Branch, Safety Officer - BP persistent cell phone (985-665-7093). 

• BP-provided Safety Officer for Houma - 985-709 5957 

• St. Petersburg, Fla., Incident Command - Fish and Wildlife Research Institute, 100 8th 

Avenue SE, St. Petersburg FL 33701, 904-755-8008

• Fish and Wildlife Service (FWS) Safety Officer, Mobile, Ala. sector

• Fish and Wildlife Service Safety Officer, Houma, La. sector

• DOI Occupational Safety and Health Manager

• USGS Bureau Industrial Hygienist 

• USGS Eastern Region Industrial Hygienist 

• USGS Bureau Watercraft Safety Program Manager, USGS Center for Coastal and 

Wetland Studies, St. Petersburg, Fla.
21 

Online resources

• Joint Incident Command: 

http://www.deepwaterhorizonresponse.com/go/doctype/2931/53023 

• DOI: http://www.doi.gov/deepwaterhorizon/, and 

https://www.smis.doi.gov/smisaux/OilSpillInfo.htm 

• USGS: http://www.usgs.gov/deepwater_horizon/

3.6.2 Waste Disposal and Other Environmental Issues 

Questions should be referred to the designated DOI IC staff at the Office of Environmental 

Policy and Compliance for Policy, Management, and Budget. Waste disposal and other 

environmental issues are covered in Section 4. 

3.6.3 Watercraft Decontamination and Vessels of Opportunity (see Section 4.2) 

• USGS personnel should notify the IC in advance regarding decontamination services for 

Water Science Center vessels: Mobile, Ala., Incident Command Center, 985-493-3343 

mc252decon@gmail.com 

• Mobile Decontamination Center, 251-455-3010 (for locations of Mobile IC Region Decon 

Centers, see www.bpdecon.com) 

• Vessels of Opportunity coordination hotline: 866-279-7983 or 877-847-7470 

3.6.4 Accident Reporting

All accidents are to be reported within the DOI Safety Management Information System (SMIS) 

accessible at https://www.smis.doi.gov/ and by clicking on the "Accident Reporting" tab. Note 

that under the "Special (Disaster Response Related) Accident Report" section, the Department 

has added the following category "During the Response to the Gulf Oil Spill." This category 

must be marked when reporting accidents involving individuals who become ill or are injured 

during natural disaster relief efforts. On the injury selection page there is an entry button that 

allows the reporting supervisor to categorize an injury. This specialized entry page has specific 

questions on PPE and training. Questions related to SMIS may be directed to the DOI 

Occupational Safety and Health Manager, 202-288-5549/202-904-0008 or USGS Headquarters 

Safety and Health Specialist, 703-648-7553. 
22 

4.0 Site Setup and Decontamination

This section provides protocols and procedures for dividing a highly contaminated site into zones 

of greater to lesser contact with hazardous substances (Section 4.1) and the procedures to be used 

to clean equipment that has been in contact with such substances (Section 4.2). Requirements for 

how to handle the decontamination of sampling equipment when working under hazardous-waste 

operations is described in Title 29 Code of Federal Regulations (CFR) 1910.120 

(http://www.osha.gov/pls/oshaweb/owadisp.show_document?p_table=standards&p_id=9765). 

This guidance specifically addresses work performed in oil-contaminated environments, such as 

those encountered in the Gulf of Mexico as a result of the Deepwater Horizon oil rig explosion. 

It is to be implemented in addition to the procedures described in chapter 3 of the National Field 

Manual (U.S. Geological Survey, variously dated) that are used routinely by USGS project 

personnel for cleaning sample-collection and sample-processing equipment. The cleaning of 

multiparameter sondes is treated separately in Section 5.0 of this report. 

The extent to which all or some of the procedures described in this guidance are implemented is

determined by the team leader or project management and depends on conditions at the site 

during field operations, the types of equipment being used, and whether or not the equipment 

will be reused at another site. The team leader must hold a current certification for the 40-hour 

Hazardous Waste Operations and Emergency Response (HazWOper) training, which qualifies 

her/him to make the appropriate onsite decisions. All decisions made and actions taken that 

deviate from the original plan are to be documented in the field logbook. 

4.1 Work Zones

Upon entering the field site, sampling and decontamination areas are delineated so that the level 

of contamination decreases at the boundaries of the work zone (fig. 4). These work zones are

defined by the level of contamination contained within their boundaries and provide the 

framework for a system of movement between and among the zones. Delineation of the work 

zones described below is adapted when sampling involves working from or on a boat. 

• The Hot Zone or Exclusion Zone (EZ) is where sample collection and processing take 

place and therefore is the zone of heaviest contamination. The EZ is designated and 

cordoned off with police tape; for example, the yellow tape shown in the photos 

(fig. 5). Personnel who enter the EZ must be properly certified, trained, and equipped, as 

described in Section 3 of this report and in the HASP (Appendix E). Sampling equipment 

and personnel move from the EZ directly to the CRZ to contain any contamination that 

was encountered. 

• The Contamination Reduction Zone (CRZ) is the area designated for the cleaning and 

decontamination of handheld equipment, including nondisposable PPE, and for disposal of 

single-use clothing and equipment. Decontamination stations are set up within the CRZ 

during site mobilization and before sampling. One person should be assigned 

responsibility for activities carried out in the CRZ. 
23 

• The Support or Safety Zone (SZ) is where field personnel put on PPE before starting 

work and where clean and decontaminated equipment and supplies are stored and 

protected from the contaminated environments of the EZ and CRZ. 

• The Contamination Reduction Corridor (CRC) is the pathway between the EZ, CRZ, 

and SZ, along which personnel move to the EZ and from the EZ to the CRZ and, after 

decontamination, from the CRZ to the SZ. Personnel entering the CRC wear the same 

level of PPE as those who work in the CRZ. Another corridor may be required for the 

entry and exit of heavy equipment. 

For sampling operations that require site access by boat, the EZ is established on the wetland or 

barrier island (fig. 5B) and a zone of initial equipment decontamination (a CRZ) and a clean 

support zone (SZ) should be established on board and delineated with police tape. (See Section 

4.2.2.2 for boat decontamination.) 
24 

Figure 4. Flowchart showing site setup for sampling and equipment decontamination.
25 

A 

 Photo by Shane Stocks, U.S. Geological Survey.

B 

Photo by Jason Griffith, U.S. Geological Survey.

Figure 5. Photographs showing the Exclusion Zone delineated by yellow police 

tape: (A) Biloxi Beach, Mississippi, and (B) wetlands at Bay Jimmy, Louisiana. 
26 

4.2 Decontamination Procedures

The purpose of decontamination is to eliminate the transfer of contaminants, including chemical 

substances and nonindigenous invasive species, between samples, sites, personnel, and 

equipment. Removing or neutralizing contaminants from equipment minimizes the likelihood of 

sample cross contamination, reduces or eliminates transfer of contaminants to clean areas, and 

prevents mixing of incompatible substances. Protocols for decontamination and disposal of PPE 

are to be included in the HASP. 

• In preparation for the site visit, all the equipment to be used for sampling that actually or 

potentially will contact the sample must be cleaned and stored according to standard 

USGS protocol (see NFM chapter 3 in U.S. Geological Survey, variously dated). This 

protocol includes the collection and analysis of equipment blanks before field work 

begins, to the extent possible. 

• Nondisposable sampling equipment and clothing (for example, rubberized waders, elbowlength rubber, and Type V Model 280 PFDs) must be decontaminated or otherwise 

cleaned appropriately after each use according to the procedures provided in this protocol. 

• In general, equipment only undergoes full decontamination at the field site if the 

equipment will be used at another site on the same day and additional sets of precleaned 

equipment are not available. To the degree practical for this project, disposable equipment 

will be used and disposable clothing will be worn to minimize the need for 

decontamination and avoid contact with caustic or volatile decontamination fluids as well 

as contaminated equipment. 

4.2.1 Cleaning Agents

Gross contamination of equipment is removed using a combination of mechanical and chemical 

methods, depending on the type of equipment, the degree to which equipment has been 

contaminated, and the sample analyses to be performed. 

1. Mechanical actions

a. Abrasive action: Abrasive materials, such as disposable metal or nylon brushes, are 

used to remove the surface layer of the contaminant. Care must be taken not to 

scratch or otherwise damage vulnerable surfaces of the equipment being cleaned.

b. Water under low or high pressure: A low-pressure water rinse using a slender nozzle 

and hose, similar to a garden sprayer, can be used onsite to spray hard-to-reach places 

in smaller equipment. High-pressure pumps flush contaminants from equipment and 

are used, generally, offsite for cleaning boats or other large equipment at pressure 

ranges from 340 to 680 atmospheric units (atm) and flow rates from 20 to 140 liters 

per minute. Pressure-rinse methods sometimes employ a low-sudsing, nonphosphate 

detergent.

c. Simple rinse: Spraying or squeezing water through a dispenser bottle is used to 

remove substances adhering to the exterior of bottles, sonde and sensor surfaces, and 
27 

equipment crevices. Contaminants are removed by dilution, physical attraction, and 

solubilization. 

d. Damp or dry cloth: Cloths are used to wipe off oily, chemical, and sediment

substances that have adhered to equipment. 

2. Chemical complex formation is used to inactivate contaminants by neutralization, 

chemical reaction, disinfection, or sterilization.

a. Chemical agents: Use of chemical cleaning agents such as hydrochloric or sulfuric 

acid and a solvent such as methanol, whether in the field or laboratory, is understood 

and familiar to USGS personnel, who should follow the equipment-cleaning protocols 

in chapter 3 of the National Field Manual. 

b. Sterilization: Equipment disinfection or autoclaving, when necessary, will be 

performed in the laboratory, following procedures given in the National Field Manual

(see NFM 7.1, http://pubs.water.usgs.gov/twri9A7/ in U.S. Geological Survey, 

variously dated). 

Additional considerations when applying decontamination methods include: 

• ASTM Type I deionized water used in cleaning/decontamination procedures must be 

verified by laboratory analysis to be below the method detection level for the 

contaminants of concern. 

• For equipment-cleaning purposes, use of an untreated potable water supply is not an 

acceptable substitute for tap water. Tap water from any municipal or industrial water 

treatment system should be of the appropriate quality. 

• To avoid possible bias to the analytical data, ensure that any residue from detergents or 

solvents has been removed completely before samples are collected with the equipment. 

See Section 4.2.4 for a list of the equipment and supplies needed for equipment 

decontamination. 

4.2.2 Contaminant Reduction Zone (CRZ): Five-Station Equipment-Decontamination Procedure 

The CRZ is arranged into a series of stations or steps that facilitate and contain the equipmentdecontamination process. The flowchart in figure 4, indicates a five-station setup in the CRZ, but 

the actual number of steps needed depends on the type and degree of contamination and the 

amount and type of equipment that has been affected, which in turn depends on the cleaning 

solutions and supplies to be used. If not dictated by an official policy, it is left to the best 

professional judgment of the field-team leader to decide whether an acid rinse and (or) methanol 

rinse is required and whether it should be performed onsite or in a laboratory. 

The information that follows about the five-station setup reflects the currently accepted standard 

operating procedure for equipment decontamination for field sites for which containment of 

hazardous waste is a factor. In this project, USGS field teams will employ single-use, disposable 

equipment in a manner that minimizes the amount of solid waste and maximizes containment of 
28 

hazardous substances and, therefore, are not expected to need the acid or methanol CRZ stations 

described below. 

4.2.2.1 CRZ Station Setup 

Begin by covering the surface of the CRZ with plastic sheeting that is sufficiently large to 

contain all decontamination equipment and supplies (for example, 4 ft by 10 ft). Set up stations 

with the equipment and supplies needed for equipment decontamination: arrange buckets, 

solutions, low-pressure sprayers, and other equipment and supplies to be used at each station. 

Typically, reused handheld sampling equipment and PPE require two to three 5-gallon buckets 

per station. Modify the CRZ setup as appropriate, depending on whether the equipment that 

requires an acid and (or) organic-solvent rinse will be decontaminated in the field or laboratory. 

If decontamination of equipment will include offsite use of acid and (or) methanol (for 

example, in an office laboratory), wash and rinse equipment as described for Stations 1, 2, 

and 3(a), and store the equipment in an extra-heavy trash bag labeled “contaminated equipment” 

for transport to the office laboratory. 

Station 1—Mechanical removal of visible contaminants: Using a brush or scraping tool, 

manually remove surface soil, such as mud or caked oil, from cleanable PPE and equipment 

(rubberized waders and gloves, buckets; any other equipment for reuse) (fig. 6). 

• Scrapings may be left onsite.

• Take care to use tools and pressure suitable for cleaning the equipment without damaging 

it.

• Discard disposable contaminated equipment (such as nitrile gloves, stakes, bucket liners, 

plastic sheeting) into properly labeled solid waste canisters or heavy trash bags and seal. 

Station 2—Wet wash: Fill a 5-gallon bucket with approximately 3 gallons of a solution of tap 

water and detergent. Use a scrub brush and the detergent solution to remove visible particulate 

matter and residual oils and grease. Rinse with potable water using a low-pressure dispenser. 

Repeat in a second bucket, if necessary. 

• Capture the waste solution in a 5-gallon container. 

• Contaminated, soapy wash water must be disposed of properly offsite to avoid bias to the 

dispersant (DOSS surfactant), nutrient, or other sample analyses. 

Station 3—Second wet wash, acid rinse, and inorganic-blank water rinse: 

a. Wet wash. Fill a 5-gallon bucket with approximately 3 gallons of tap water and use a 

clean, well-rinsed scrub brush to clean equipment a second time. Follow this by rinsing 

thoroughly with deionized water, using a low-pressure dispenser. Capture the waste 

solutions in a 5-gallon container for proper offsite disposal. (Skip to Station 3 step (c) if 

no acid rinse is needed. If an acid or organic-solvent rinse will be performed offsite, skip 

to Station 5).

b. Acid (or bleach) rinse. To remove inorganic constituents and bacterial DNA, acid-rinse 

the equipment. Wear gloves appropriate for contact with acidic or caustic solutions. Pour 
29 

a 5-percent hydrochloric acid (pH less than or equal to 2) or a 10-percent bleach solution 

into an uncolored plastic basin for a 15- to 30-minute equipment soak (if needed) or rinse 

equipment by dispensing the acid or bleach solution through the nozzle of a 

squirt/squeeze bottle. If equipment requires soaking for contaminant removal, follow with 

a squirt-bottle-dispensed rinse. Capture all the waste solution in an acid-waste designated 

container for proper offsite disposal. 

• Bleach option: Use a freshly opened bleach container. 

• Thorough removal of any acid or bleach residue is essential to maintain the integrity of 

the samples. 

c. Blank-water rinse. Complete the work at this station by rinsing equipment thoroughly 

using laboratory-certified inorganic-grade blank water7

 (IBW) dispensed under low 

pressure. Repeat the IBW rinse at least five times, capturing rinsate in the designated 

labeled container for offsite disposal. (If a methanol rinse will not be needed, repeat the 

IBW rinse two times, followed by a VOC- and pesticide-grade blank water (VPBW) rinse 

repeated three times; skip to Station 5).

Station 4—Solvent (methanol) and organic-blank water rinse: 

a. Methanol rinse. Wear gloves appropriate for contact with organic solvents. To remove 

trace organic compounds, dispense laboratory-grade methanol or other organiccompound solvent from a Teflon squirt/squeeze bottle or wipe equipment down 

thoroughly using clean, organic solvent-wetted cloths. Place equipment on an aluminum 

foil-covered tray and allow the solvent to evaporate completely from the equipment. 

Capture liquid methanol waste in an appropriate container and keep it capped. Dispose of 

methanol-wetted cloths in a metal canister and keep the canister capped. 

b. Deionized- and blank-water rinses. Fill a 5-gallon bucket with approximately 3 gallons 

of deionized water and scrub methanol-rinsed equipment with a clean brush. Next, fill a 

low-pressure rinse dispenser withVPBW and rinse equipment, capturing the rinsate in an 

organic-solvent storage canister for proper offsite disposal. 

Station 5—Disposable equipment and PPE: Remove and discard disposable PPE, along with 

any disposable sampling-related equipment into a labeled rubbish can lined with a heavy-duty 

trash bag and seal it shut. 

On-Board Stations—Equipment cleaning on boats: Sampling operations that require boataccess to a site at which it is not practical to establish on-land decontamination zones must plan, 

at the least, for on-board equipment cleaning procedures as described above for Stations 1 and 2. 

The boat must be set up with a clearly defined clean (SZ) zone and cordoned decontamination 

(CRZ) zone. After completing the Station 1 and 2 cleaning, the rinsed equipment is packed into 

 

7 USGS personnel obtain certified inorganic- and organic-grade blank water through the USGS One Stop Shop.
30 

labeled heavy-duty plastic trash bags for transport to the onshore decontamination station. 

Completion of decontamination procedures should be executed at the boat launch or later at 

appropriate office facilities. 

TAKE NOTE! Liquid and solid wastes from decontamination efforts must be containerized in 

appropriate and labeled containers and disposed of in accordance with the prevailing State, 

local, or Federal regulations. Unified Command decontamination stations normally will accept 

properly containerized waste. 

Figure. 6. Photograph showing the decontamination of waders at Station 1 in the Contamination Reduction Zone. Photograph 

by Jason Griffith, U.S. Geological Survey. 

 
31 

4.2.2.2 Boat Decontamination

A decontamination plan must be in place when a boat (or other large equipment) is required for 

sampling in oil-contaminated waters. Boats can be decontaminated offsite at IC/UC

decontamination staging stations or onsite by the field team. 

USGS Water Science Centers may decide to use Bureau watercraft or contract for the use of 

privately owned boats, known as Vessels of Opportunity (VOO). USGS personnel are 

responsible only for decontamination of USGS vessels. This is most conveniently accomplished

at IC/UC-operated staging stations, if available. The UC or IC should be contacted in advance of 

the field work to arrange for vessel decontamination at such staging stations. These stations often 

are mobile land or water operations whose locations can change throughout a day or week. To 

arrange for boat decontamination for this project:

• Contact the Houma IC Decon Center, 985-493-3343, mc252decon@gmail.com, or the 

Mobile IC Decon Center, 251-455-3010, depending on the sector in which you are 

working. You will be directed to the nearest decontamination center. 

• Information for finding VOO is available through the VOO Hotline, (866) 279-7983, 

(877) 847-7470, or by contacting the VOO Program Coordinator for Houma, La., at 427-

773-9983 (check the current Shift Plan for contact names and numbers). 

It is recommended that Bureau watercraft be pressure-rinsed with clean water and allowed to dry 

before mobilizing offsite, to prevent the spread of contaminants. Under some circumstances, 

allowance may be obtained for boats to be cleaned at a car wash after the field team completes 

onsite removal of oil, flora, and fauna. 

Onsite boat decontamination by the USGS field team is to be avoided. Use IC decontamination 

stations, if possible. For onsite boat decontamination: 

• Set up a decontamination pad. The decontamination pad consists of a bermed area of 

appropriate size to the equipment to be decontaminated, lined with 2 layers of 10-mil

plastic sheeting. Berms may be constructed of 2-in. by 6-in. lumber, and the pad should 

contain a low spot or sump from which fluids can be pumped into the required containers 

for disposal (properly labeled Department of Transportation (DOT) rated containers) and 

subsequently transported to the IC Decontamination Station or other regulated facility that 

accepts hazardous waste. 

• Prepare a soapy solution of potable tap water and surfactant detergent, such as Liqui-Nox 

or Dawn, and scrub large surfaces. Rinse with tap water under pressue. If necessary, wipe 

with methanol-wetted disposable cloths, then discard as hazardous waste.

• A gas-powered steam cleaner can be used on boats or any other large, heavy equipment 

while on the decontamination pad. 
32 

4.2.3 Post-Decontamination Procedures

Questions and general guidance with respect to the containment and disposal of hazardous waste 

materials should be directed to the local USGS safety officer, Bureau Safety officer, or the 

Safety Officer of the National Water Quality Laboratory.

1. For waste solutions generated in a high-pressure pad area (for example, onsite boat 

decontamination): 

a. Collect liquid waste from the high-pressure pad and heavy-equipment 

decontamination area and store in appropriate drum or container. A sump pump can 

aid in the collection process. Refer to the DOT requirements for appropriate 

containers based on the contaminant of concern. 

b. Collect solid waste from the high-pressure pad and heavy-equipment decontamination 

area and store in appropriate drum or container. Refer to the DOT requirements for 

appropriate containers based on the contaminant of concern. 

2. Detergents: Empty soap-and-water liquid wastes from basins and buckets and store in 

appropriate drum or container. Refer to the DOT requirements for appropriate containers 

based on the contaminant of concern. 

3. Acid solutions: Empty acid-rinse waste and place in appropriate container or neutralize 

with a base, such as marble chips or baking soda, and place in appropriate liquid-waste 

drum. pH paper or an equivalent pH test is required to ensure that the neutralization 

threshold of pH 6 or greater has been achieved. 

4. Organic solvent (methanol): Empty methanol-rinse sprayer and methanol waste into the 

appropriate container, such as an empty container in which it originally was contained at 

the time of purchase. Consult DOT requirements for appropriate drum for solvent-rinse 

waste.

5. Low-pressure sprayers, rinse basins, and brushes: Place liquids generated from this 

process into the wash-water rinse container. 

6. Place all solid waste materials generated from the decontamination area (gloves and 

plastic sheeting, etc.) into an approved DOT drum. Refer to the DOT requirements for 

appropriate containers based on the contaminant of concern. 

7. Label waste containers and make arrangements for disposal. Consult DOT regulations for 

the appropriate label for each drum containing waste that was generated from the 

decontamination process. An IC/UC staging station may be available for waste disposal.
33 

4.2.4 Equipment 

The materials and tools listed below (also listed in Appendix B) are recommended for the 

decontamination procedures described above. 

Decontamination Reagents and Solutions

• Nonphosphate detergent, such as Liqui-Nox or Dawn

• A 5-percent hydrochloric acid solution in a rinse bottle (for inorganics) 

• A 10-percent fresh bleach solution to submerge Teflon handheld equipment 

• Laboratory-grade methanol in Teflon rinse bottle (for organics) 

• Tap water (with and without detergent) in 5-gallon buckets and spray bottle 

• Deionized water in 5-gallon buckets and inorganic blank water (IBW) and volatilepesticide-grade organic blank water (VPBW) in dedicated spray bottles/garden sprayers 

• Marble chips or baking soda (for acid neutralization) 

Decontamination Tools/Supplies

• Long- and short-handled brushes

• Bottle brushes 

• Drop cloth/plastic sheeting 

• Kimwipes, oil-absorbent cloths (such as WypAll X70), paper towels

• 5-gallon buckets with handles and lids 

• Disposable noncontaminating (Teflon) 5-gallon bucket liners 

• Aluminum foil, heavy duty 

• Low-pressure washer; squeeze/squirt bottles – polyethylene and Teflon 

• High-pressure washer

Health and Safety Equipment 

• Health and Safety PPE, as described in Section 2.4 and modified in the HASP 

• Copy of the HASP 

• Material Safety Data Sheets (MSDS) for all cleaning and decontamination agents to be 

used

• Police tape to establish EZ and CRZ boundaries 

Waste Disposal 

• Trash bags, heavy duty 

• Trash containers 

• Department of Transportation (DOT)-certified metal/plastic containment canisters or 

drums for transportation and storage of decontamination solutions and liquid waste 

• Labels to identify the nature of the waste
34 

5.0 Multiparameter Sondes: Preparation, Deployment, and Cleaning 

Procedures

Data collection for the USGS Deepwater Horizon post-landfall sampling project includes 

measurement of ambient physical and chemical properties of water at specified locations in

nearshore and wetland environments of the Gulf of Mexico. This section of the sampling 

protocol addresses the special preparation and cleaning procedures needed for multiparamter 

sondes that might be immersed in saline, oil-laden waters, and to the protocols and procedures 

for sonde deployment and measurement of water properties. This section assumes a working 

knowledge of the standard USGS protocols for field measurements found in chapter 6 of the 

National Field Manual for the Collection of Water-Quality Data (see U.S. Geological Survey, 

variously dated). 

Measurements of in situ water-quality properties employ multiparameter instruments containing 

data sondes attached to multimeter data output and recording devices. Temperature, specific 

electrical conductance/salinity, pH, and dissolved-oxygen concentration/percent saturation (by 

luminescent optical sensor) are required measurements for the USGS Deepwater Horizon Oil 

Spill 2010 investigation. Field-measurement sensors are to be calibrated onsite, following 

calibration methods and requirements described in the NFM, section 6.8 of chapter 6. 

The effects of oily water on the response and sensitivity of multiparameter instrument sensors 

may vary somewhat, depending on the instrument in use. The YSI 6-series instrument is used for 

illustrative purposes in this guidance. Other equipment manufacturers may have slightly different 

procedures to address deployment of their instruments in oil-laden waters (Appendix G includes 

information provided by In Situ, Inc. in addition to that provided by YSI, Inc.). 

5.1 Sonde Preparation

Sonde preparation focuses on the special considerations and procedures required for the 

deployment and decontamination of multiparameter sondes in an oily saltwater environment. A 

list of the materials and supplies recommended for sonde cleaning and deployment can be found 

at the end of this section and in Appendix B. 

The instrument type and the date, time, and method of calibration should be recorded in the field 

logbook; calibrations are recorded on field forms and in the meter calibration logbook, including 

a post-sampling calibration check. 

• In situ field properties should be measured at the same location at which the water samples 

will be collected.

• Measurements should be completed before collecting the samples for laboratory analysis. 
35 

The YSI company recommends the following procedure before deploying the multiparameter 

sonde in an oil-contaminated environment: 

1. Apply C-Spray nanopolymer protective coating to exterior of YSI instrument, sensors, 

and cable, according to the YSI instruction sheet8

 (Appendix G). (YSI reports that testing 

has demonstrated that C-Spray has no negative effect on YSI optical sensors, ROX 

membranes, or YSI pH sensors.). 

2. YSI ROX DO sensor: Spray and disperse C-SprayTM over membrane and sensor face. 

Allow to sit 5 minutes. Wipe excess spray off with a Kimwipe.

3. YSI pH: Spray sensor body including bulb and junction area. Allow to sit for 5 minutes. 

Shake off any excess spray.

4. All other optical sensors: Remove wiper, spray C-Spray onto sensor face and wait for 5 

minutes. Remove excess with Kimwipe and polish sensor face with dry Kimwipe to 

remove streaking. Inspect wipers and replace or reinstall. 

5. Calibrate the sensors after the C-Spray application, using standard USGS procedures 

(NFM 6.8). 

5.2 Methods for Sonde Deployment 

Three methods for sonde deployment are outlined in the subsections that follow. The method 

selected depends primarily on the presence and thickness of product on the water surface and on 

surf conditions: 

• Water surface with no visible oil or a light sheen; calm or active surf conditions. 

• Water surface with definite oil sheen, distributed oil pods (for example, as “mousse” or 

“pancake” pods), or light sheen; more active sea conditions.

• Water with heavy, measurable oil layer and/or active or rough sea conditions. 

The same criteria are used when selecting a sampling method, as described in Section 6. Section 

6 also contains the step-by-step instructions for collecting in situ water properties and samples.

Field teams should expect surf conditions to be rougher than they appear; for this reason the 

PVC-tube method for handling the sonde (Section 5.2.3) is recommended in all but reliably calm 

conditions to help manage and control the distance of the sonde above the seabed. 

5.2.1 Direct-Dip (Sorbent-Sweep) Method 

Use: No oil or light oily sheen. This method parallels the direct-dip method for collecting water 

samples described in Section 6.4.3. 

 

8 Do not use C-Spray on instruments from other manufacturers without first consulting with that manufacturer.
36 

While wearing appropriate PPE: 

1. Clear the water surface by gently sweeping the surface with a disposable absorbent cloth 

to avoid dispersing surface oil into the water column. 

2. Discard the soiled absorbent into a contaminant-designated trash bag. 

3. Lower the sonde into the cleared water column per the step-by-step procedures given in 

Section 6.4 for conducting a profile and record of field measurements. 

4. Remove the sonde and rinse it with distilled/deionized water (DI water). Store it safely 

until it can be cleaned (refer to Section 5.3). 

5.2.2 Plastic Bag Method9

Use: Noticeable surface sheen, continuous “oil mousse,” or widely distributed pods 

(“pancakes”) of oily product on the water surface. (See Section 5.2.3 for an alternative to this 

method). The plastic bag method parallels the peristaltic-pump (or bailer) method used for 

sample collection, but also can be used if samples will be collected using the direct-dip method 

(see Section 6.4.3). Refer to the diagrams that illustrate this method in Appendix G. 

1. Place sonde in a clean, disposable plastic bag, covering the entire sonde. 

2. Cut out the bottom of the bag. 

3. Use rubber bands to close the bag above and at the bottom of the sonde. 

4. Place a third rubber band around the bag and body of the sonde, above the sensors. 

5. If feasible, avoid deploying sonde through oil. Alternatively, gently clear the oil layer 

from the water surface with a disposable absorbent cloth, taking care to avoid dispersing 

surface oil into the water column. Drop the soiled cloth into a trash bag for contaminated 

waste.

6. Deploy the sonde vertically below the oil layer.

7. Carefully clear any surface oil again (see step 5) before inserting gloved hands and arms 

into the water. Expose the measurement sensors. Remove the lower rubber band; fold the 

bag up to, and secure it with, the rubber band near the center of the sonde. 

8. Follow the step-by-step “Sampler 1 – Sampler 2” procedures described in Section 6.4.3 

for conducting a measurement profile and recording the field measurements. 

9. Detaching the bag from the center rubber band, lower the bag back over the sensors to 

avoid contact with product. Raise the sonde out of the water. 

10. Remove the bag and dispose of it in a trash bag designated for contaminated waste. Wipe 

down the elbow-length, rubber-coated gloves and discard them along with the wipe in the 

contaminated-waste trash bag, or remove and store them in a dedicated trash bag for 

subsequent decontamination. 

11. Rinse the sonde with DI water and store safely until it can be cleaned (Section 5.3). 

 

9 The plastic bag method for sonde deployment was adapted from procedures recommended by YSI, Inc.
37 

5.2.3 PVC Tube Method 

Use: In an active surf, or measurable thickness of free product, or densely distributed oil 

“pancakes.” This method parallels the peristaltic pump or bailer method for collecting water 

samples, described in Section 6.4.2, and requires installation of a stabilizing stake to which the 

PVC tube is secured. Note that when working in deep wetland or marsh mud, the weight of the 

tube can cause progressive sinking of the stake, making this method difficult to carry out or 

requiring modification of the method to better suit site conditions.

1. Install the PVC tube; refer to Section 6.4.2 for detailed instructions. 

2. Lower the sonde through the PVC tube, avoiding contact with product. 

3. Follow the step-by-step procedures given in Section 6.4 for developing a profile and 

record of field measurements. 

4. Remove the sonde from the tube. 

5. Rinse the sonde with DI water and store safely until it can be cleaned (Section 5.3). 

5.3 Instrument Decontamination

Crude oil is thick and sticky and may affect the performance intervals of the sensor membranes 

and wipers on multiparameter instruments, in comparison with normal conditions. The YSI 

company has provided the following instructions for cleaning YSI 6-seriesTM multiparameter 

instruments that become contaminated with crude oil (Appendix G). Section 5.4 lists the 

materials and supplies recommended for sonde and sensor cleaning. This procedure should be 

carried out in the CRZ. 

5.3.1 Cleaning Procedure

1. Wear gloves and eye protection when handling items contaminated with crude oil. 

2. Spray all contaminated areas with a degreasing agent, such as Simple Green®, for 

removal of surface contamination. 

3. Use a soft cloth or paper towels to remove excess oil from the sonde. Remove oil-coated 

wiper pads and brushes from sensors in accordance with the manufacturer’s instructions 

and discard. Work carefully when cleaning around sensors, membranes, or glass 

components. 

4. Submerge instrument in a bucket filled with warm, soapy water.

5. Use a soft brush to wipe away remaining oil. 

6. Use a small brush to clean the inside of the cell containing the temperature and 

conductivity sensors. 

7. Discard water, rinse bucket thoroughly, and refill the bucket with soapy water. Rinse the 

sonde and sensors in soapy water.

8. Repeat steps 5 through 7 as many times as is necessary to remove oily residue.
38 

9. Rinse again, in a fresh container of warm, soapy water. Rinse soap residue off of the 

sonde and sensors using clean tap water followed by DI water. 

10. Dry the sonde gently. 

11. Install new wiper pads and brushes, as instructed by the instrument manufacturer. 

12. Discard oily water and oil-saturated wipers, brushes, and cloths in proper receptacles and 

in accordance with local regulations for hazardous materials.

13. Check the calibration of the sensors. 

5.3.2 Decline in Sensor Sensitivity

The most common problems related to oil coating of sensors will be addressed by adhering to the 

steps for cleaning the sonde and sensors described above. However, the pH, depth, and 

dissolved-oxygen (luminescent/optical) sensors may require additional attention, as described 

below (contact the sonde manufacturer if additional guidance is needed): 

• pH: The performance of the pH and pH/ORP (oxidation-reduction potential) sensors relies 

on the sensitivity of the glass bulb and reference junction. The pH sensor may require 

additional cleaning in warm (35°C) soapy water while stirring the solution rapidly. 

• ROX DO Membranes: The DO membrane on the luminescent/optical sensor also 

benefits from being cleaned with a warm, soapy water solution. Stirring or gentle sweeps 

with a soft paint brush across the membrane should aid in cleaning. The calibration of the 

DO sensor should be checked periodically against a Winkler titration. 

• Depth: Spray Simple Green into depth-port openings and use pipe cleaners to remove any 

visible dirt or contaminant.

5.4 Materials and Supplies for Sonde and Sensors Cleaning and Preparation

• Health and safety PPE, as described in Section 3.4 and modified for site-specific health 

and safety plans (Appendix E–2). 

• Field- (onsite) calibrated multiparameter water-quality meter and sonde 

• YSI C-Spray nanopolymer coating 

• Calibration solutions and Winkler titration kit

• 2- to 3-ft-long by 4-in. inside diameter PVC tube (through which a sonde can fit) 

• 5- to 6-ft-long metal or wooden stake to stabilize the PVC tube

• Plastic bag to cap water end of the PVC tube during tube installation 

• Replacement sensor brushes and wipers; hex wrench

• Heating plate, magnetic stirrer, and stir bars

• Rubber bands, extra strength 

• Gloves 
39 

• Buckets

• Soft-bristle brushes, soft paint brush, pipe cleaners, and Q-tips 

• Lint-free, laboratory-grade cloths, such as Kimwipes, for delicate membranes

• Heavy-duty disposable absorbent towels, such as WypAll X70 wipers, for oil removal

• Liqui-Nox, Dawn, or other effective, nonphosphate detergent liquid 

• A degreaser, such as Simple Green 

• Waste-collection containers, heavy-duty trash bags, and extra disposable plastic bags 
40 

6.0 Collection of Field Measurements and Water Samples

The protocols described in this section were developed to assist field personnel in collecting 

water data and samples in the marine nearshore environment during USGS post-landfall 

sampling in the Gulf of Mexico, and should be used in addition to the standard procedures 

described in the National Field Manual (U.S. Geological Survey, variously dated) chapter 4, 

“Collection of Water Samples” and chapter 5, “Processing of Water Samples”. Chain-of-custody 

requirements will be followed strictly in the collection, processing, transport, handling, storage, 

and documentation of the samples and data collected. 

6.1 Objectives and Method Overview

A primary goal of the post-landfall sampling effort is that the sample data accurately represent 

the ambient water properties at the given sampling location at the time of sample collection. To 

achieve this goal it is important that the data assembled during post-landfall sampling are 

collected using USGS methods and protocols consistently among all sampling sites and field 

teams, to the degree possible and as appropriate for site conditions. However, field teams will 

exercise professional judgment to determine the most appropriate method for the given field 

conditions. Owing to the complexity of the planned sampling operations, the large variety and 

types of samples to be collected, and the potentially hazardous conditions that might affect health 

and safety when working in spill-impacted areas, a three-person field team is recommended 

strongly for collection of water samples; the third person will be needed to facilitate the 

transfer of samples to shore and other onshore activities; a fourth team member might be 

required if a boat is used for access to the sampling site. 

Selection of sampling method depends on site conditions at the time of sampling, including the 

presence, extent, and thickness of floating product. This protocol defines two methods as 

preferred for collecting water samples under anticipated sampling conditions in the Gulf of 

Mexico: 

• Direct-Dip Method: This method is used to collect samples when no oil is visible on the 

water surface or when a slight oil sheen is observed that easily can be removed for the 

duration of field-measurement data and sample collection. 

• Peristaltic-Pump Method: This method should be selected for sampling under conditions 

when free product either is observed in the area where samples will be collected or is close 

enough so that it could intrude into the sampling location during field measurements and 

sample collection. The method involves installation of a PVC tube affixed to a stake 

through which the multiparameter sonde and pump tubing can be deployed. 

An alternative to the peristaltic-pump method—the disposable-bailer method—is provided in 

Section 6.7. Field teams might elect to use the bailer method if it better fits the logistics of the 

field conditions encountered. 
41 

6.2 Equipment and Supplies 

Cross-contamination problems are eliminated or minimized for this project by using dedicated, 

disposable sampling equipment to the extent possible. The sampling methods described require 

different sets of equipment. Selection of the sampling device should be based on its potential 

effect on the analyses to be performed. The equipment selected is to be certified as appropriate 

for its intended use, meaning that it is demonstrated that the equipment can not itself be a source 

of the analytes targeted for study. Equipment certification for this purpose is accomplished 

primarily by the use of equipment blanks, which are collected and analyzed before field work for 

the project begins, and that includes quality assurance of new, in addition to previously used, 

equipment (see Section 9). All equipment, whether disposable or nondisposable (reusable), is to 

be cleaned and quality assured with an equipment blank before its first field deployment, in 

accordance with the protocols and procedures outlined in the National Field Manual and this 

report. This requirement does not apply to equipment that has been quality assured or precertified by a laboratory, such as bottles for organic-compound analyses. Tables 1 and 2 detail 

the containers and some key supplies to be used for water sampling during this project (see also 

Appendices B and D). 

Contrary to standard USGS procedure, hydrochloric acid (HCl) will not be added in the 

field to the volatile organic compounds (VOC) sample for this project. VOC samples will be 

stored on ice and shipped to the TestAmerica Laboratory overnight on the day of collection to 

ensure that the 7-day maximum holding time for unacidified VOC samples is met. Adding acid 

to seawater samples with high carbonate concentration can result in either an immediate or 

delayed effervescence, potentially compromising the representativeness of the VOC analysis. 
42 

Table 1. Containers and preservatives specific to water-column sampling. 

[mL, milliliter; HNO3, nitric acid; CIN, laboratory’s analytical identification number; TAL, TestAmerica Laboratory; H2SO4, sulfuric acid; oz, 

ounce; HCl, hydrochloric acid; VOA, volatile organic analysis; BTEX, benzene toluene ethylbenzene xylenes; L, liter; TPH GRO, total 

petroleum hydrocarbons – gasoline-range organics; DRO, diesel-range organics; SVOC TCL, semivolatile organic compounds target compound 

list; NWQL, National Water Quality Laboratory; DOSS, di(ethylhexyl) sodium sulfosuccinate; DOC, dissolved organic carbon; One Stop-NFSS, 

U.S. Geological Survey’s National Water Quality Laboratory One-Stop Shopping–National Field Supply Service] 

Containers Specific to Water-Column Sampling1

Sample container and

chemical preservative

Analysis

Laboratory

Source of 

container

One 250-mL wide-mouth 

polyethylene bottle. Contains 

HNO3 

Total metals2 - CIN 50017 (Method 6020)

TestAmerica, Pensacola, Florida (TAL)

TAL

One 250-mL wide-mouth 

polyethylene bottle, brown. 

Contains H2SO4 

Total Kjeldahl Nitrogen - CIN 50068 (TKN, Method 351.2) 

Total Ammonium

Total Phosphorus – CIN 50092 (TP, Method 365.4)

TestAmerica, Pensacola, Florida 

TAL

One 32-oz, fired glass, widemouth jar. Contains HCl

Oil and Grease - CIN 50136 (Method 1664A)

TestAmerica, Pensacola, Florida

TAL

Two VOA vials, 40 mL, 

no preservative

VOC, BTEX - CIN 50109 (Method 8260B)

TestAmerica, Pensacola Florida 

TAL

Two VOA vials, 40 mL, 

no preservative

TPH GRO - CIN 50114 (Method 8015B)

TestAmerica, Pensacola, Florida 

TAL

One 1-L, fired, amber glass, no 

preservative 

TPH DRO - CIN 50130 (Method 8015B)

TestAmerica, Pensacola, Florida 

TAL

Two 1-L, fired, amber glass, 

no preservative

SVOC TCL,- CIN 50117 (Method 8270D)

TestAmerica, Pensacola, Florida 

TAL

Two 1-L Teflon bottles, no 

preservative

DOSS (Surfactant) 

NWQL, Denver, Colorado (E. Furlong)

NWQL, 

precleaned

One 125-mL, fired amber 

glass bottle, DOC

Dissolved Organic Carbon, field filtered

USGS, Boulder, Colorado (G. Aiken)

One Stop-NFSS

One 1-L polyethylene bottle, 

acid-rinsed 

Sampling device for collection of samples for trace metals and 

nutrients into pre-preserved TAL containers

One Stop-NFSS

One 500-mL, fired amber 

glass

Sampling device to collect whole water to be filtered for DOC One Stop-NFSS

1

Add the extra sample containers needed when the work schedule calls for collection of quality-control samples. 2

Analyses include: Sb, As, Ba, Cd, Cr, Co, Cu, Pb, Mn, Mo, Ni, Se, Ag, Tl, Zn.
43 

Table 2. General supplies for water-column sampling.

[DOC, dissolved organic carbon; DO, dissolved oxygen; SC, specific electrical conductance; PPE, personal 

protective equipment; HCl, hydrochloric acid; N, Normality; ASR-CoC, Analytical Services Request and Chain of 

Custody form; ft, foot; in., inch; mil, millimeter] 

Supplies Specific to Water-Column Sampling1

Equipment Description Use

Flotation device; 

backpack; coolers

Device, such as an inner tube into which coolers can be 

inserted and floated to shore; or, backpack or fielddetermined alternative.

Transport bottles to shore

Filter Pall AquaPrep disposable disk filter. DOC 

Disposable towels Kimwipes or WypAll X70 cloths. Oil removal 

Peristaltic pump and 

pump tubing

Dedicated, disposable precleaned, precut 8-ft or greater 

lengths of C-Flex tubing. 

Sampling method and DOC 

sample filtration

Bailers (optional) 1.5-in. diameter, Teflon, pressurizable, disposable. Sampling method

PVC tube 4-in. diameter, from 1.5 ft to 5 ft in length. Sampling method

Tape measure; 

Wading rod 

1/10 of a ft graduated. Water column measurement

Survey markers Stakes, flags, or buoys and anchors. Stake out location

Multiparameter 

sonde and Winkler

DO kit

pH, luminescent DO, SC/salinity, temperature sensors; 

calibration solutions, including Winkler kit.

Field measurements of water 

properties

Gloves Rubber-coated outer gloves, elbow length (minimum two 

pair per sampler) – nondisposable.

Nitrile inner gloves, (minimum five pair per sampler per 

site) – disposable.

Water sampling PPE

Adhesive tape Teflon, Duct, Electrical. Seal sample caps/lids

pH test strips pH test papers (for example, pHydrion papers). Check pH of oil and grease

HCl ampoules 6 N HCl ampoules (extra). Oil and grease preservation

PPE See Section 3, “Safety.” Personal safety 

GENERAL USE

• Photoionization detector (vapor analyzer) 

• 2-pound sledge hammer; hose clamp(s)

• 4-ft (or longer) wooden (disposable) or metal 

stakes (one per site if disposable)

• Deionized water in spray bottle

• Ziploc bags 4-mil gauge; leak-proof coolers

• Industrial-strength rubber bands

• ASR-CoC and Field forms (Appendix F)

• Wet ice and Dry ice; Trash bags, heavy duty

• Aluminum foil to wrap Teflon-bottle samples

1

Supplies for the collection of water quality-control samples are listed in Section 6.5.1.1. Refer to Appendix B for a compiled list 

of equipment and supplies.
44 

6.3 Sampling Location 

Water samples for this project will be collected in nearshore waters of the Gulf of Mexico and its 

barrier islands and wetlands. Sampling and site conditions of the Gulf Coast vary widely; 

however, the general criteria that influence the selection of the specific sampling location at a 

field site for this investigation include:

• The sampling location should be the same as, or close to, a pre-landfall sampling location 

(Appendix A), unless samples will be collected to meet an objective different than those 

for the pre-landfall effort (for example, collection of tarballs). 

• The location is representative of observable physical and chemical conditions at the site. 

To this end, samples will be collected to represent “normal” surf and suspended sediment 

conditions at the time of sampling.

• Samples are to be collected in wadeable water deep enough so as to minimize 

resuspending bed sediments; for example, from about 2 to 3 ft deep. 

• Samples should be collected at mid-depth of the water column, at 15 cm (0.5 ft) or more

above the seabed to avoid entraining suspended sediments. 

• Samples should be collected at 15 cm (0.5 ft) below a surface oil layer and in a manner 

that avoids collection or incorporation of free product in the sample, unless the sample is 

being collected for oil analysis. 

• Sampling locations at barrier islands will be accessed by boat, but samples generally 

should not be collected from the boat unless necessary to maintain sample integrity.

Working in wetlands having deep, mucky sediments might require sampling from a boat if 

personal safety is at stake. 

6.4 Step-By-Step Procedures

Step-by-step procedures are given below, according to the sonde-deployment and samplecollection method that is determined by the field team as most appropriate for the onsite 

conditions observed (fig. 7). Field teams should customize the procedures given as best meets 

their need and in accordance with their professional judgment and maintenance of scientific 

integrity; however, each team must record in the logbook the modified procedure used and, to 

the extent reasonable, use the same procedure for each of their sampling sites. Field personnel 

will follow standard National Field Manual protocols for checking, preserving, handling, 

and maintaining sample integrity, unless otherwise stipulated in this sampling protocol 

(U.S. Geological Survey, variously paged). Upon collection and during transport, all samples 

will be kept chilled or frozen, in accordance with the laboratory instructions for the sample type. 

The temperature of chilled samples is not to exceed 4oC (39.2oF). All samples will be packaged 

and shipped for priority overnight delivery and be in compliance with strict Chain of Custody 

(CoC) dictates.
45 

Figure 7. Flowchart showing water-column sampling, Gulf of Mexico Deepwater Horizon oil spill, 2010.
46 

The protocol for determining representative field measurements of temperature, pH, specific 

electrical conductance/salinity, and dissolved oxygen (DO) is the same as prescribed in the 

National Field Manual (refer to chapter 6 in U.S. Geological Survey, variously paged), with the 

caveat that the DO reading in Gulf water should be checked against the results of a Winkler 

titration at least once for each Water Science Center field team. After each field deployment, 

check the sensor calibration and record the results. Table 3 is adapted from a similar table in the 

National Field Manual that provides the stabilization criteria for determing the final field 

measurements to be recorded as representing site conditions. In addition to the field 

measurements that will be recorded as representative of the water column for a given site, 

readings should be recorded at several points in the water-column profile to document the 

occurrence of stratification. 

Table 3. Stabilization criteria for field measurements. 

In situ field measurement Stablization criteria1 

Temperature 

(Thermistor thermometer )

± 0.2°C (degrees Celsius)

Specific Electrical Conductance 

> 100 μS/cm (microsiemens per centimeter)

± 3 percent of five or more measurements

Salinity (Conductivity sensor) Greater of: ± 1 percent of reading or 0.1 ppt (parts per thousand)

pH ± 0.2 pH unit 

Dissolved oxygen (DO)

(Luminescent optical sensor )

± 0.2 mg/L (milligrams per liter)

1 The variability of the measurement should be within the criterion value shown for five or more measurements.

6.4.1 Preparation and Order of Sample Collection

Preparing to collect samples:

1. Put on Tyvek apparel. 

2. Prepare a water bucket for post-use of the multiparameter sonde (Section 5.0), and have 

available waste containers and Kimwipes or absorbent cloths (absorbents) for oil 

skimming (if needed).

3. Assemble field-measurement and sampling equipment according to the method selected 

(Direct Dip or Peristaltic Pump). 

4. Complete labels on all bottles with indelible (non-fume-producing) ink (site, time, date, 

and analysis) and tape labels to bottles with wide clear tape (2-in. width). Appendix D 

Table D–1 describes the containers, preservatives, holding times, and laboratory 

requirements for each aliquot. 

5. Pack sample bottles and sampling equipment in a floating cooler, backpack, or other 

device to transport samples to shore. Line the floating cooler, backpack, or other sampletransport device with a large plastic bag into which sample containers are placed. 
47 

6. Wear PFDs, three layers of inner nitrile gloves (or as determined by the field team), outer 

rubber-coated elbow- (or full-arm) length gloves, and other PPE, as appropriate. 

7. Record and characterize the presence of free product, such as oil sheen, the extent of 

floating product, and the estimated diameter(s) and distribution of the surface oil.

a. Determine the sonde-deployment method to be used: (1) Direct Dip, (2) Plastic Bag, 

or (3) PVC Tube (recommended when sampling in active surf). 

b. Determine the sampling method to be used: (1) Direct Dip or (2) Peristaltic 

Pump/PVC Tube (alternatively, Disposable Bailer). 

8. Calibrate sonde sensors as prescribed in the National Field Manual, chapter 6, section 

6.8 (see U.S. Geological Survey, variously dated). Prepare the sonde for oil immersion 

before starting measurements, according to the instructions given in Section 5.0. 

9. Using a two-person team in proper PPE, wearing rubber outer and inner gloves, wade to 

the sampling location. 

10. As a rule of thumb, collect samples consistently with respect to wave or current direction; 

that is, with ebb or flow. Record the procedure used. 

11. When sampling at heavily oiled, deep-mud, or slick-surface locations, the safety of 

personnel must take priority, possibly necessitating sample collection from the boat 

instead of wading. Take the precautions needed to avoid becoming immobilized in deep 

mud. Avoid resuspending bed sediment.

12. Collect organic vapor readings with a PID, in the breathing zone and 6 in. above the 

water surface at the sampling location. Record readings on field forms or in the project 

logbook. 

13. Record GPS location in the field logbook and on the field forms. 

14. Measure and record to the nearest tenth of a foot the wave height and depth of the water 

column. If possible, depth of the water column should be from 2 to 3 ft.

Order of sample collection: 

1. Field measurements: PID, oil thickness, and in situ water-quality properties 

2. Volatile Organic Compounds – VOCs

3. Total Petroleum Hydrocarbon compounds – Gasoline Range (TPH-GRO)

4. Total Petroleum Hydrocarbon compounds – Diesel Range (TPH-DRO)

5. Semivolatile (SVOC) Polycyclic Aromatic Hydrocarbon (PAH) compounds 

6. Surfactants – di(ethylhexyl) sodium sulfosuccinate (DOSS) 

7. Trace metals/elements 

8. Nutrients 

9. Dissolved Organic Carbon – DOC

10. Oil and Grease

6.4.2 Peristaltic Pump Method

This method is selected when a definite sheen or measurable free product is observed. 
48 

• For samples to be analyzed at the TestAmerica Laboratory (TAL) in Pensacola, Fla., 

sample bottles for oil-and-grease, metals/trace-element, and nutrient analyses will be 

supplied that already contain the chemical preservative needed for the intended analysis. 

• A portable peristaltic pump with battery can be transported in a sidepack or backpack to 

the sampling location by Sampler 1, while Sampler 2 transports and manages the sample 

bottles. 

• The step-by-step procedure that follows describes use of a PVC tube through which the 

multiparameter sonde and peristaltic pump tubing are deployed. 

• Maintaining the appropriate distance of the PVC tube above seabed may be difficult in 

soft wetland mud; if the tube is too heavy (too long), it can sink into the muck. Modify the 

length of the tube or the procedure as needed. 

To collect samples using the peristaltic pump method:

1. Install the PVC tube 

a. Drive a 5- to 6-ft stake 1 to 2 ft or more into the bottom material with the sledge 

hammer.

b. Cover the bottom end of the PVC tube with a plastic bag.

c. Lower the plastic-covered end of the PVC tube through the water surface, keeping it 

at least 1.5 ft above seabed and ensuring that product does not get inside the tube. 

Fasten the tube to the stake using Velcro straps or cable ties. 

d. Remove the protective plastic bag from the end of the PVC pipe. 

2. Field measurements 

a. The multiparameter sonde must have been calibrated and prepared per Section 5 of 

this document and in accordance with USGS standard protocols (NFM chapter 6, 

section 6.8).

b. Lower the sonde through the PVC tube to approximately mid-depth of the water 

column, but at least 0.5 ft above seabed. 

c. Measure and record the depth of sensors below the water surface to one-tenth of a 

foot. 

d. Check for stratification within the water column by recording measurements at about 

0.5 ft above and below the “mid-depth” site measurement, if possible. Be sure to keep 

the sonde at least 0.5 ft above seabed to avoid contact with suspended sediment.

e. Move the sensors to mid-depth of the water column. Employing NFM protocols, 

record stabilized measurements for pH, SC/salinity, DO, and temperature (table 3) on 

field forms. This comprises the record of in situ measurements for this site. Check the 

DO value of the Gulf water against a Winkler titration at one sampling site.

f. Remove the sonde from the PVC pipe for a calibration check of the sensors. Store the 

sonde in clean potable water until the appropriate decontamination or cleaning 

process can be completed (see Section 5).
49 

3. Prepare sampling equipment (do not field-rinse containers)

a. Sampler 2: Remove the protective wrap from the intake end of the disposable, 

precleaned pump tubing and lower tubing through the PVC tube to the desired depth 

for sample collection. 

b. Sampler 1: Adjust and secure the location of the tubing intake end. Wipe down and 

remove rubber-coated elbow- or arm-length gloves; discard wipe and disposable 

gloves in the trash bag or container dedicated to such waste; store reusable gloves and

soiled equipment in appropriately labeled containers for subsequent decontamination. 

c. Sampler 2: Wearing nitrile gloves, turn on the pump and adjust it to a slow but steady 

rate of flow. Circulate water for a 3-volume tubing field rinse. 

4. Collect VOC and TPH-GRO samples 

For VOC samples  use 2 VOA vials. For TPH-GRO  use 2 VOA vials.

a. Sampler 1: Uncap the first VOA vial and hold it for Sampler 2. 

b. Sampler 2: Fill VOA vial and cap to overflowing, leaving a meniscus in both. 

c. Sampler 1: Pour water from cap into VOA vial while capping the vial, so as to 

exclude air and prevent bubbles from forming. Cap VOA vial; invert and tap vial to

check for bubbles. If bubbles are observed, uncap vial and repeat steps 4b and c until 

no bubbles are observed. 

d. Sampler 1 and 2: Repeat steps 4 a – c until the 4 VOA vials have been collected 

successfully. 

e. Sampler 2: Clean and dry each vial, ensure cap is on securely, wrap or place vials in 

foam sleeves, place in doubled ziploc bags, and store on ice in the appropriate cooler 

with a trip blank (vial caps should be sealed using Teflon tape when back on shore). 

5. Collect TPH-DRO and SVOC samples (adapt the Sampler 1 – Sampler 2 technique but 

leave at least 1 inch of headspace) 

a. Sampler 1: Fill one 1-L glass amber bottle for TPH-DRO and hand to Sampler 2. 

b. Sampler 1: Fill two 1-L glass amber bottles for SVOC, handing each to Sampler 2.

c. Sampler 2: Dry each container, check labels, ensure cap is securely tightened, place 

glass containers in foam or bubble sleeves, place each sample container in doubled 

ziploc bags, and store on ice in the appropriate cooler. 

6. Collect Surfactant (DOSS) samples 

a. Two 1-L Teflon for Surfactant (USGS-NWQL).

b. Using the same Sampler 1 – Sampler 2 technique, fill the first Teflon bottle to threequarters of capacity to allow for expansion when frozen. Cap it securely and repeat 

this procedure with the second Teflon bottle. 
50 

c. Sampler 2: Dry each bottle, ensure cap is securely tightened, check label, wrap in 

aluminum foil and then into doubled ziploc bags. Store on dry ice or in wet ice until 

samples can be frozen and placed in the appropriate cooler. 

7. Collect Total Metals/Trace Element and Total Nutrient samples, adapting the 

Sampler 1 – Sampler 2 technique as follows 

a. Sampler 1: Fill a 250-mL pre-preserved polyethylene bottle for Total Metals/Trace 

Elements and a 250-mL brown polyethylene bottle for Total Nutrients, leaving at 

least one-half inch of headspace and taking care to prevent loss of the preservative. 

Hand each sample bottle to Sampler 2. 

b. Sampler 2: Dry each container, check labels, and ensure that the cap is securely

tightened. Invert each bottle at least three times to distribute the preservative. Place 

each sample container in doubled ziploc bags and store on ice in the appropriate 

cooler. 

8. Collect the DOC sample 

a. Sampler 1: Wearing clean gloves unwrap the AquaPrep filter and secure it onto the 

pump tubing. 

b. Sampler 2: Uncap and hand the 125-mL baked glass for DOC to Sampler 1. 

c. Sampler 1: Pass about 50 mL water through the filter before filling the DOC bottle to 

the shoulder. Cap the filtered sample and hand it to Sampler 2. 

d. Sampler 2: Dry the bottle, check label, ensure the cap is securely tightened, place into 

foam sleeve, then into doubled ziploc bags, and store on ice in the appropriate cooler.

e. Sampler 1: Turn off the pump and discard tubing and used filter into a dedicated 

waste receptacle. 

9. Collect the Oil and Grease (O&G) sample by the Direct-Dip Method

a. Sampler 1 and 2: Put on long rubber gloves over nitrile gloves. 

b. Sampler 2: Uncap and hand a 1-L HCl-preserved O&G sample container to Sampler 

1. 

c. Sampler 1: Skim sample from the water surface into the HCl-preserved container 

carefully, capturing surface oil but taking care not to lose the HCl preservative (if 

possible), and leaving about 1 inch of headspace. Hand container to Sampler 2.

d. Sampler 2: Recap and wipe the container clean to remove oily product. Check that 

the lid is secured tightly and that the container is marked with the type of preservative 

to ensure proper labeling. Invert three times to mix. Place into bubble or foam sleeve 

and then into doubled ziplock bags. Store on ice. 

e. Sampler 1, 2, or 3: Once on shore, if you suspect that preservative was lost, check the 

sample pH by decanting a small amount of sample and estimating pH with a pH strip. 

If pH is greater than 2, add contents of a HCl ampoule (2 mL of 6N HCl) and record 
51 

this information in the logbook. Rewrap the O&G container, tape the lid, and place on 

ice.

10. Sampler 2: Remove the stake and PVC tube and return to the decontamination area

(CRZ). A wooden stake can be discarded as solid hazardous waste; the PVC tube either is 

similarly discarded or contained for decontamination. 

11. Sampler 1: Secure all samples and return to shore. Decontaminate sample coolers and the 

equipment used to bring the samples to shore. 

12. Samplers 1, 2, and/or 3: Ensure that lids are appropriately taped and containers are 

properly labeled and protected in foam or bubble sleeves. Pack bottles in appropriate 

shipping coolers, in dry ice or wet ice, as instructed by the laboratory, and ship by

priority overnight or following day delivery to the respective laboratories. Check sensor 

calibration after cleaning the multiparameter sonde.

6.4.3 Direct-Dip Method

The direct-dip method consists of collecting water samples directly into the precleaned sampling 

containers at a predetermined depth below the water surface (Natural Resource Damage 

Assessment and Restoration Program, 2010). Procedures for measuring in situ water properties 

and collecting samples are given below. In the sampling scenario, Sampler 1 collects the water 

samples. Sampler 2 manages the sampling containers before and after the sample is collected. 

The following description of the general procedure to be used is a departure from NFM 

methods—please read carefully: 

TestAmerica Laboratory (TAL) in Pensacola, Fla., supplies sample bottles for oil and grease, 

metals/trace elements, and nutrient analyses that already contain the chemical preservative 

needed for the intended analysis. To prevent loss of preservative, samples for metals/trace 

element and nutrient analyses will not be collected directly into the TAL-provided preservativecontaining sample bottle (“preserved containers”). Instead, a 1-L polyethylene RA (“raw 

acidified”) bottle, precleaned by the field team, will be used as the sampling device. Water is 

poured from the RA bottle into the appropriate TAL-supplied preserved containers. This 

eliminates the need for field personnel to add the chemical preservatives needed to the samples 

for metals and nutrient analyses. 

1. Field Measurements. When in low-energy surf, use the Direct-Dip Method or Plastic

Bag Method; for high-energy surf, the PVC-Tube Method is recommended. (Use

professional judgment to evaluate field conditions and make sampling decisions.) 

a. The sonde must have been calibrated and prepared per Section 5 of this document and 

in accordance with USGS standard protocols (NFM 6.8). 

b. Lower the water-quality sonde to the sampling depth (follow Plastic Bag procedures 

in Section 5.2.2 if this method is to be used before deploying the sonde). 

c. Measure and record depth of sensors below the water to one-tenth of a foot. 

d. Check for stratification within the water column by recording measurements at about 

0.5 ft above the seabed and below the water surface “mid-depth” site measurement, if 
52 

possible. Be sure to stay at least 0.5 ft above seabed to avoid contact with suspended 

sediment.

e. Move the sensors to mid-depth of the water column and, using NFM protocols, record

on field forms the stabilized measurements for pH, SC/salinity, DO, and temperature. 

This comprises the record of in situ measurements for this site. Check the DO value 

of the Gulf water against a Winkler titration at one of the sampling sites.

f. Remove the sonde from the water and check the calibration of the sensors. Store the 

sonde in a bucket of clean water until it can be cleaned properly. 

2. Prepare to collect water samples (do not field-rinse sample containers)

a. Sampler 1: With rubber outer and inner gloves on, clear the sampling area of any 

surface oil by carefully sweeping the area with Kimwipes or sorbent towels, such as 

WypAll X70, and discard absorbents in dedicated trash bag. 

b. Sampler 1: Remove outer gloves and store in reusable storage bag for 

decontamination. 

3. Collect VOC and TPH-GRO samples (2 VOA vials per analysis)

a. Sampler 2 hands Sampler 1 capped VOA vials, one at a time.

b. Sampler 1: Submerge first VOA vial to the appropriate depth (between 0.5 ft and 1 ft 

below the water surface), uncap the vial until full, then recap under water. 

c. Sampler 1: Remove VOA vial from the water, invert the VOA vial, tap the bottom of 

the vial, and check for bubbles. If bubbles are observed, resubmerge the capped vial, 

uncap the vial allowing all bubbles to escape; repeat until no bubbles are observed. 

d. Sampler 1: Repeat steps 3a and b with the next three VOA vials.

e. Sampler 1: Hand each completed VOA vial to Sampler 2. 

f. Sampler 2: Double check for bubble; if bubble is present, repeat the sampling (steps b

and c) process. Dry each vial with a clean absorbent towel; check to make sure the 

lids are tight and the sample is properly labeled. Place the vials in foam or bubble 

sleeves, double-bag in ziplocks, and store on ice with a trip blank. (Vial caps should 

be sealed with Teflon tape here or when back on shore.) 

4. Collect TPH-DRO, SVOC samples

a. Sampler 2 gives Sampler 1 the 1-L glass amber container for TPH-DRO. 

b. Sampler 1: Submerge the capped container to the appropriate depth, uncap and fill 

until full; recap the container and bring to the surface. Hand to Sampler 2. 

c. Sampler 2: Hand the capped container to Sampler 1. Dry, place in foam or bubble 

sleeve, double bag and store on ice. 

d. Sampler 1: Repeat steps 4a through c to collect the SVOC samples. 

e. Sampler 2 hands Sampler 1 the 1-L bottle for SVOC, followed by the second 1-L 

SVOC/PAH bottle, and repeats steps a through c for each SVOC 1-L container. 
53 

f. Samper 2: Once on shore, uncap the TPH-DRO and SVOC containers and decant 

sample to within about 1 inch of the top to leave room for expansion when chilled. 

Recap securely, wipe the containers clean and dry, secure the lid with Teflon tape, 

and check that the container is labeled properly. Replace the containers in a bubble or 

foam sleeve and double-bag the samples. Store on ice. 

5. Collect Surfactant (DOSS) samples (no container field rinse)

a. Sampler 2 hands Sampler 1 the 1-L Teflon bottles, one at a time.

b. Sampler 1: Submerge the capped Teflon bottle to the appropriate depth, uncap, and fill 

to three-quarters of capacity to allow expansion when frozen (decant excess water 

above the water surface, if necessary, to leave sufficient headspace). Recap the 

container and bring to the surface. Hand to Sampler 2. 

c. Samper 2: Decant some sample, if necessary. Recap, wipe the container clean and dry, 

check to make sure the lid is tight and the container is labeled properly, wrap in 

aluminum foil, double bag in ziplock bags, and store on ice or dry ice (Appendix D, 

Table D–1),

d. Sampler 1 and 2: Repeat steps 5b and c with the second Teflon bottle. 

6. Collect Metals/Trace Elements and Nutrients 

a. Sampler 2 hands Sampler 1 an NWQL 1-L RA bottle, precleaned and qualitycontrolled at the Water Science Center, for use as a sample-collection device. 

b. Sampler 1:

i. Field rinse: Submerge the capped RA bottle and uncap. Allow a sufficient 

volume of water to enter the bottle. Cap the bottle and bring it above the water 

surface to field rinse. Repeat this rinse procedure two more times. 

ii. Collect sample: Submerge the capped RA bottle and uncap. Fill the bottle to 

near the top. Recap the container and bring to the surface. 

c. Sampler 2: Uncap a TAL 250-mL HNO3-preserved container for metals analysis.

d. Sampler 1: Uncap the RA bottle. Carefully decant sample from the RA bottle into the 

HNO3-preserved 250-mL container being held by Sampler 2, leaving about 1 inch of 

headspace. Recap the RA bottle.

e. Sampler 2: Cap the HNO3-preserved 250-mL container, wipe the container clean and 

dry, check that the lid is tight and the container is labeled properly for HNO3

preservative, and store on ice in a protective wrap.

f. Sampler 2: Uncap a TAL 250-mL H2SO4-preserved container for nutrients (TKN, 

NH4, and TP) analysis.

g. Sampler 1: Uncap the RA bottle. Carefully decant sample from the RA bottle into the 

H2SO4-preserved container being held by Sampler 2, leaving headspace. Discard any 

remaining sample from the RA bottle.
54 

h. Sampler 2: Cap the H2SO4-preserved container. Wipe the container clean and dry, 

check that the lid is tight and the container is labeled properly for H2SO4 preservative, 

and store on ice in a protective wrap. 

7. Collect DOC sample (no container field rinse) 

Sampler 2 hands Sampler 1 an NWQL-fired 500-mL amber bottle labeled “TOC.” 

a. Sampler 1: Submerge the capped NWQL bottled to the appropriate depth, uncap and 

fill until almost full. 

b. Sampler 2: Secure AquaPrep filter to the discharge end of the pump tubing. Hand 

inlet end of tubing to Sampler 1. 

c. Sampler 1: Insert pump tubing into 500-mL DOC sampling container, and turn pump 

on at a low pump rate. Pass three tubing volumes of sample through the tubing for a 

field rinse; attach the filter and pass about 50 mL of sample water through the filter. 

d. Sampler 2: Uncap the preserved DOC bottle. After tubing and filter field rinse, hold 

the discharge end of the filter over the DOC bottle and fill to shoulder. Recap firmly. 

Wipe the container clean and dry, check that the lid is tight, check that the “DOC” 

label is intact, and store on ice in a protective wrap. 

e. Sampler 1: Shut down the pump and discard extra sample to its source. Remove and 

discard pump tubing and RA sampling bottle. 

8. Collect Oil and Grease (O&G) (no container field rinse) 

a. Sampler 1 and 2: Put on long rubber gloves over nitrile gloves. 

b. Sampler 2: Uncap and hand a 1-L HCl-preserved O&G sample container to Sampler 

1. 

c. Sampler 1: Skim sample from the water surface into the HCl-preserved container 

carefully, capturing surface oil but taking care not to lose the HCl preservative and 

leaving about 1 inch of headspace. Hand container to Sampler 2. 

d. Sampler 2: Recap and wipe the container clean to remove oily product. Check that 

the lid is secured tightly and that the container is marked with the type of preservative 

to ensure proper labeling. Invert three times to mix. Place into bubble or foam sleeve 

and then into doubled ziplock bags. Store on ice. 

e. Sampler 1, 2, or 3: Once on shore, if you suspect that preservative was lost, check the 

sample pH by decanting a small amount of sample, estimate the pH using a pH strip; 

if pH > than 2, add a contents of an HCl ampoule (2 mL 6N HCl) and record this 

information in the logbook. Rewrap the O&G container, tape the lid, and place on ice.
55 

9. Float or backpack/shoulder-pack the samples to shore, taking precautions to prevent Gulf 

water from wetting the samples. (Line cooler or backpack(s) with doubled clear trash 

bags into which samples are placed as collected; end collection by tying the bags closed).

10. Check sensor calibration after cleaning the multiparameter sonde.

6.5 Quality Control for Water Samples

Provide quality control (QC) in the field for samples collected by each Water Science Center 

(WSC) engaged in the response to the 2010 Deepwater Horizon oil spill in the Gulf of Mexico. 

QC sample types to be collected include field (ambient) blanks, replicates, and matrix spikes for 

the sample types indicated below (Section 7 provides information about quality-control sample 

types for sediment analyses). Samples will be bottled in accordance with the laboratory 

requirements. Table D–1 in Appendix D provides the laboratory requirements for water 

samples.When collecting QC samples, the standard USGS parts-per-billion and cleanhands procedures and precautions are to be followed (NFM chapter 4, section 4.3 in U.S. 

Geological Survey, variously dated), in addition to the following caveats: 

• All sampling equipment is to be precleaned according to USGS protocols (NFM chapter 3

in U.S. Geological Survey, variously dated) and quality assured by collecting equipment 

blanks according to USGS protocols (NFM chapter 4; see also Section 9 of this report). 

Laboratory-certified blank water, including volatile- and pesticide-compound-grade 

deionized water (VPBW) and inorganic-analyte-grade deionized water (IBW) is obtained 

through the USGS National Field Supply Services (One-Stop Shop). 

• To quality assure the equipment used for the peristaltic-pump sampling method: 

− Lengths of sample tubing are cut, prepared, and dedicated to one field site; 

− Each length of tubing must be thoroughly cleaned before use per NFM 3 procedures; 

− The tubing must not come in contact with methanol; 

− Each WSC collects an equipment blank for one length of tubing. 

• Use the TAL-supplied sample bottles with preservative (“pre-preserved” containers) for 

the respective metals/trace-elements, nutrients, and oil/grease samples. 

• As soon as possible, and before starting sampling at the first site, collect an equipment 

blank (tubing blank) for each of the analyses shown below (also shown in Appendix D, 

Table D–1). Ship equipment-blank samples to the respective laboratories immediately, 

requesting a quick turnaround. Collection of an equipment blank is a one-time requirement

for each of the coastal Water Science Centers (unless laboratory results indicate a qualityassurance problem). 

• For this project, it will not be necessary to use an enclosed (sample-processing) chamber 

when collecting field blanks. Field blanks should be exposed to onsite atmospheric 

conditions; that is, they are all ambient blanks (the length of atmospheric exposure should 

mimic the environmental sampling process). On the other hand, equipment blanks should 

be collected within an enclosed chamber or glove box in the office laboratory. 
56 

• Ensure that sample bottles or any other of the supplies, equipment, or materials to be used 

in the field have not come in contact with or proximity to methanol. Methanol storage and 

use, either onsite, during transport, or in the office, must be completely sealed and 

separated from sampling equipment and supplies. A logbook entry should document how 

methanol isolation has been accomplished. 

• Samples for VOC analyses will be collected in duplicate in VOA vials, instead of in 

triplicate. 

6.5.1 Blank Samples

Each Water Science Center should process one complete set of equipment blanks once before 

environmental sampling begins. Equipment-blank samples should be collected in a sampleprocessing chamber, using IBW for inorganic sample analyses and VPBW for organic sample 

analyses, as appropriate. 

6.5.1.1 Equipment Blanks

Equipment blanks are prepared in the office laboratory under clean and controlled conditions. 

The equipment blanks are to be collected well before project field work begins to allow time for 

these samples to be analyzed by their respective laboratories and for the results to be evaluated. 

Should laboratory results indicate the presence of a constituent or compound that is targeted for 

study, the Water Science Center team first should consult with other Centers engaged in this 

project to determine if similar problems have been found. The field team is accountable to 

review their cleaning and sampling procedures, how the equipment was handled and stored, 

repeat the cleaning and blanking procedure for each piece of equipment separately, and review 

analytical results for the new set of equipment-blank samples until they are satisfied that they 

understand and have solved the problem. These requirements are described in NFM chapter 4.3. 

When collecting equipment blanks, follow standard USGS protocols and procedures (NFM 

chapter 3) to clean sample tubing, containers for unfiltered (raw) acidified samples (RA bottles), 

and disposable filters. Put on nitrile gloves and rinse gloved hands three times with about 1 L of 

IBW. Change gloves with each major change in procedure. Leave sufficient headspace in each of 

the samples being collected and refer to Appendix D, Table D–1 for preservation and shipping 

requirements. Referring to Appendix D, Table D–1: 

• TAL analyses

1. Pump three tubing volumes of IBW through tubing as an initial rinse; then fill the RA 

bottle.

− Pour IBW sample from RA bottle into one 250-mL polyethylene container 

acidified with HNO3 for metals analysis.

− Pour IBW sample from RA bottle and into one 250-mL polyethylene container 

acidified with H2SO4 for nutrient analysis. 

2. Pump three tubing volumes of VPBW through tubing. Collect: 

− VOC and GRO samples in 40-mL vials, two vials per sample.

− TPH-DRO sample in 1-L amber glass container.
57 

− SVOC sample in two 1-L amber glass containers.

− Oil & Grease sample in 1-L clear, widemouth glass container. 

• NWQL Denver surfactant analysis—Fill 1-L Teflon bottle with VPBW. 

• USGS-Boulder DOC analysis: 

− Within processing chamber, attach AquaPrep filter to pump tubing. 

− Rinse filter with 50 mL of VPBW. 

− Collect VPBW in 125-mL amber DOC bottle. 

Equipment-Blank Supplies

• 1-L acid-rinsed (RA) bottle from NWQL Oil Spill Kit*

• C-flex tubing, approximately 8 feet in length* 

• Pall AquaPrep filter from NWQL Oil Spill Kit*

• Portable peristaltic pump 

• Nitrile gloves

• Inorganic Blank Water (IBW) (estimate three bottles)

• Organic Blank Water (VPBW) (estimate four 12-L bottles)

• 125-mL DOC bottle from NWQL Oil Spill Kit

• 1-L Teflon bottle from NWQL Oil Spill Kit

• 250-mL HNO3-preserved bottle from TAL site-sample set

• 250-mL H2SO4-preserved bottle from TAL site-sample set

• For cleaning solutions and solution-treatment and disposal materials, refer to Appendix B. 

* Equipment for which an equipment blank is planned. 

6.5.1.2 Ambient Field Blanks 

Select the site at which to collect one complete set of ambient field blanks. Ambient blanks 

should be collected before collecting environmental samples and while at the sampling location, 

as follows: 

1. Check and apply labels – the container (bottle) for each blank analysis requires a unique 

sample ID that must appear on the container label and be recorded on the CoC form, 

using the same procedure as for an environmental sample. 

2. Purge peristaltic pump tubing with three tubing volumes of freshly opened, laboratorycertified, Volatile/Pesticide-grade Blank Water (VPBW).

3. Ambient Blank for VOCs – Check PID measurements. An ambient blank should be 

collected once per day at field sites where PID measurements exceed a reading of 15 

ppmv total VOCs in the Exclusion Zone. 

• Fill two VOA vials and caps to overflowing with VPBW for VOC analysis and two 

VOA vials for TPH-GRO analysis. 
58 

• Cap securely, invert, tap, and check for gas bubbles. Check sample and hand bubblefree sample to partner. 

• Partner checks labels, packages sample, and chills samples in the same manner as 

environmental VOC and TPH-GRO samples.

• Ship overnight, with a TAL-provided trip blank, on the same day as sample 

collection.

4. Fill the remaining organic-sample containers – except for DOC – with VPBW. Pass 

completed sample set to partner to check caps/labels, wrap, and place on ice in the 

appropriate cooler.

5. DOC – Rinse the tubing by passing one tubing volume of VPBW to waste. Install the 

AquaPrep filter and field rinse by passing about 50 mL of VPBW through the filter to 

waste. Fill an unpreserved DOC bottle with VPBW. Do not preserve this sample. Pass 

to partner to check cap and label, wrap, and place on ice in the cooler for the USGS 

Boulder, Colo., laboratory. 

6. Remove and store the filter and tubing into clean, colorless ziplock bags, keeping them 

clean for later filtration of the environmental sample for DOC analysis. 

7. Purge peristaltic pump tubing with three tubing volumes of freshly opened, laboratorycertified, Inorganic-grade Blank Water (IBW).

8. Fill the set of inorganic-sample bottles with IBW, using the TAL pre-preserved bottles in 

the following order: 

• Nutrients (TKN, NH4, and total P). 

• Total metals/trace elements. 

9. Pass inorganic samples to partner to check caps/labels, wrap, and place on ice in the 

appropriate cooler.

10. Ensure that a TAL-provided temperature blank are included in every cooler that is 

shipped to TAL. 

6.5.2 Replicate Samples and Matrix Spikes

Water samples for matrix-spike, duplicate, and triplicate analyses are collected sequentially, as 

described below. Sequential replicates (duplicate and triplicate samples) consist of samples 

collected one after the other close in time and space. Consult Appendix D for preservation and 

shipping requirements that apply to this project specifically. 

Ensure that the correct QC method code is on the Analytical Services Request (ASR) form 

specifically designated for QC samples. If more than one QC sample is included, distinguish 

with time steps. 

Sites designated for collection of duplicate, triplicate, and matrix-spike samples

• Duplicates – for TAL samples only. Collect one set of duplicates per WSC, per site type 

(beach and wetland).
59 

• Triplicates – for all Research and TAL samples. Triplicates are collected only at oiled 

sites. Collect one set of triplicates per WSC, and for only one site type (beach or wetland). 

• Matrix spikes – for TAL spiking and analysis. Matrix spikes are collected only at nonoiled (“clean”) sites. Collect one set of matrix spikes per WSC, per site type (beach and 

wetland), for the following analyses: 

− SVOC, water sample: 2 extra 1-L amber bottles needed for matrix-spike analysis. 

− TPH-DRO, water sample: 2 extra 1-L amber bottles needed for matrix-spike analysis. 

Procedure for Replicate and Matrix-Spike Sample Collection

1. Collect the environmental sample first, followed immediately by collection of a set of 

duplicate samples at one beach and one wetland site, for TAL analyses only. 

a. At a clean (non-oiled) beach and wetland site, collect matrix-spike samples for TPHDRO and SVOC analyses by TAL.

b. At one oiled site only, collect a set of samples in triplicate for analyses by TAL and 

all the USGS research laboratories. 

2. Follow identical sample-collection procedures for the replicate and matrix-spike samples 

as for the environmental sample, but ensure that the samples are properly labeled and 

coded for sample type (environmental, duplicate, or matrix spike): 

• VOC/BTEX (no preservative). 

• TPH (GRO Carbon 6 to Carbon 10) (no preservative). 

• TPH-DRO  add matrix-spike sample (MS/MSD) collected at one non-oiled beach

site and one non-oiled wetland site (no preservative). 

• SVOC (no preservative)  add matrix-spike sample (MS/MSD) collected at one 

non-oiled beach site and one non-oiled wetland site.

• Total metals/trace elements (pre-preserved bottle). 

• Nutrients (TKN, total ammonium, and total P) (pre-preserved bottle). 

• Oil & Grease (pre-preserved bottle). 

• DOC (filtered, no preservative). 

6.6 Sample Handling and Storage

Once all samples have been collected:

1. Tape caps and check labels on the sample vials/bottles (containers) as instructed in 

Appendix D, table D–1. Check that cap is fastened securely. 

2. Wipe any petroleum or mud off the outsides of the containers and place the full 

containers into bubble envelopes, then double bag in ziplock bags, place on ice, protect 

from contact with ice meltwater, and place in the appropriate shipping coolers. 

3. Record collection of sample on multiple ASR forms to manage the chain of custody in 

individual coolers to the appropriate laboratories (refer to Table D–1 in Appendix D).
60 

ASR forms should be sealed in doubled ziplock bags and taped to the inside lid of the 

respective cooler.

4. If feasible, take photos of the containerized, labeled samples. 

5. Chain of Custody: Follow the detailed instructions given in Section 8. 

• Remember to record all pertinent data in the project logbook and on the appropriate 

field form(s) and sign them.

• Be sure to attach custody seals to the cooler prior to shipment.

6.7 Addendum: Disposable-Bailer Sampling Method

The disposable-bailer method may serve as a suitable alternative to the peristaltic-pump method, 

depending on site conditions. It requires repeated deployment of the disposable Teflon bailer. In 

the case where the PVC tube has been deployed, 1.5-in.-diameter disposable bailers may be used 

to collect water samples through the PVC tube, instead of using the peristaltic-pump method. 

Use bailers with sealable tops (pressurizable type) that allow the bailer to remain closed while 

being submerged to the depth of sample collection. 

The bailer is deployed after completing field-measurement procedures for sites with floating 

product, with Sampler 1 collecting the water samples and Sampler 2 managing the sample 

containers/bottles before and after the each sample is collected in its appropriate container. 

Sample containers for organic-compound analyses and bottles that contain preservative are not 

field rinsed. For this method the RA sample-collection bottle is not necessary, as the sample is 

discharged directly from the bailer into the HNO3-preserved container for metals analysis and 

into the H2SO4-preserved container for nutrients analysis. 

1. Sampler 1 and Sampler 2: Remove outer and inner rubber gloves and collect samples 

wearing inner nitrile gloves. (Each sample collector wears three pairs of inner nitrile 

gloves.) 

2. Sampler 2: Remove the disposable bailer from its sealed bag and store the release valve 

in a safe, clean location for easy access. Sampler 2 puts a clean aluminum foil swatch 

over the upper pressure port on the bailer and adds a short “leash” with a loop to attach to 

the wrist of Sampler 1. 

3. Sampler 1: Submerge the bailer to sampling depth, keeping the top pressure port covered 

using a plastic bag secured by a rubber band to the bailer, to ensure that only water from 

the chosen sampling depth enters the bailer. At the chosen depth, remove the bag and 

open the pressure port to allow water to enter the bailer. 

4. Sampler 1: Raise the bailer out of the water and present the lower water inlet/outlet port 

to Sampler 2, while keeping the upper pressure port sealed. 

5. Sampler 2: 

a. Prepare to collect two VOC and two TPH-GRO samples. Attach or insert VOA 

sampling attachment to bailer outlet port (Sampler 1: keep upper pressure port 

sealed). 
61 

b. Sampler 2: Uncap first VOA vial and place under outlet port. 

c. Sampler 1: Open pressure port to fill VOA vial and cap to overflowing, leaving each 

with a meniscus. 

d. Sampler 2: Empty water from cap into VOA vial while capping the vial, so as to 

prevent bubbles from forming. Cap VOA vial, invert and tap vial, and check for 

bubbles. If bubbles are observed, Sampler 2 will uncap vial, collect additional water 

from bailer in cap, and repeat step 5d until no bubbles are observed. 

e. Samplers 1 and 2: Repeat steps 5a – d until the four vials for VOC and TPH-GRO 

analyses have been collected successfully. 

f. Sampler 2: Clean and dry each container, ensure cap is on securely, place them into

foam or bubble sleeves, place then into doubled Ziploc bags, and store on ice in the 

appropriate cooler. Remove vials and seal caps with Teflon tape when on shore; 

replace vials into their protective sleeves, ziplock bags, and ice. 

6. Sampler 1: Repeat steps 3 and 4 as needed before continuing to Step 7. 

7. Sampler 2: Uncap, place under outlet port, and fill (leave headspace) and cap the 

following bottles to within 1 inch of the top while Sampler 1 opens the pressure port and 

fills: 

a. one 1-L baked amber glass bottle for TPH-DRO. 

b. two 1-L baked glass bottles for SVOC. 

8. Sampler 2: Clean and dry each container, ensure cap is on securely, wrap in bubble or 

foam sleeve, place in doubled Ziploc bags, and store on ice in the appropriate cooler. 

9. Sampler 1: Hand Sampler 2 the first of two 1-L Teflon bottles for the surfactant sample. 

a. Sampler 2: Uncap and place under outlet port while Sampler 1 opens the pressure 

port. 

b. Fill the bottle to two-thirds of capacity to leave room for expansion of the sample 

when frozen. Recap the bottle securely, place in foam or bubble sleeve, and place on 

ice.

c. Samplers 1 and 2, repeat steps a and b with the second Teflon bottle. 

10. Sampler 1: Hand Sampler 2 the 250-mL HNO3-preserved polyethylene container for 

Total Metals/Trace Elements. 

a. Sampler 2: Uncap, place under outlet port. 

b. Sampler 1: Open the pressure port. Fill container carefully, leaving headspace and 

avoiding loss of preservative. Recap and hand to Sampler 2. 

c. Sampler 2: Dry the container, check that container is labeled to indicate HNO3

preservative, and check that cap is securely tightened. Invert three times to mix, place 

into doubled ziplock bags, and store on ice. 

11. Sampler 1: Hand Sampler 2 the 250-mL H2SO4-preserved polyethylene container for 

Nutrients (TAL). Samplers 1 and 2 follow the same procedures as described in Step 10. 
62 

12. Samplers 1 and 2: Prepare to collect the 125-mL baked-glass DOC sample by installing 

the AquaPrep filter onto the bailer outlet. Field rinse the filter (but not the bottle) by 

passing about 50 mL of sample through the filter. Then fill the DOC bottle to the 

shoulder with sample filtrate, cap securely, place bottle into bubble or foam sleeve, then 

into doubled ziplock bags, and store on ice. 

13. Remove and discard bailer in dedicated waste receptacle. 

14. Oil and grease is collected by the direct-dip method (no container field rinse): 

a. Samplers 1 and 2: Put on long rubber gloves over nitrile gloves. 

b. Sampler 2: Uncap and hand a 1-L HCl-preserved Oil and Grease sample container to 

Sampler 1. 

c. Sampler 1: Skim or scoop sample from the water surface into the HCl-preserved 

container carefully, capturing surface oil but taking care not to lose the HCl 

preservative (if possible), and leaving about 1 inch of headspace. Hand container to 

Sampler 2. 

d. Sampler 2: Recap and wipe the container clean to remove oily product. Check that the 

lid is secured tightly and that the container is marked with the type of preservative to 

ensure proper labeling. Invert three times to mix. Place into bubble or foam sleeve 

and then into doubled ziplock bags. Store on ice. 

e. Samplers 1, 2, or 3: Once on shore, if you suspect that preservative was lost, check 

the sample pH—decant a small amount of sample, check pH with a pH strip; if pH is 

greater than 2, add a vial of 6 N HCl and record this information in the logbook. 

Rewrap the O&G container, tape the lid, and place on ice. 

15. Remove the wooden (or metal) stake and PVC tube and return to the decontamination 

(CRZ) area. Discard the stake and PVC tube into appropriate receptacles for hazardous 

waste.

16. Secure all samples, returning to shore. Decontaminate sample coolers and equipment 

used to bring the samples to shore. 

17. Pack bottles in appropriate shipping coolers, in dry ice or wet ice, as instructed by the 

laboratory, and ship for priority overnight delivery to the respective laboratories. 
63 

7.0 Sediment Samples

Standard and project-specific procedures are described in this section that will be used for 

collecting samples of sediment or other solids from an oil-impacted shoreline environment. 

These procedures are intended to be implemented in addition to standard USGS sampling and 

quality-assurance protocols as described in the National Field Manual (refer to NFM chapter 8 in

U.S. Geological Survey, variously dated). Chain of Custody (CoC) requirements will be 

followed explicitly for the collection, processing, transport, handling, storage, and 

documentation of the samples and data collected. 

The type of sediment deposits characteristic of a given sampling location influences its 

susceptibility to oil-related contamination. Moreover, differences in sediment types correspond 

with various interferences and matrix effects that can bias laboratory analyses. Contaminants are 

more likely to be concentrated in finer-grained sediments and in sediments having high organicmaterial content. Organic-rich sediments are typical of wetland areas, in contrast to the typically 

coarser and “cleaner” sediments found on beaches and in other erosional zones. The particle size 

and organic content of the sediments are related directly to the velocity and flow characteristics 

of the water body in contact with site sediments. A description of the sediment deposits and 

profile observed at the sampling site should be recorded in the project logbook with respect to 

relative particle size, sorting, and the presence of either naturally occurring or anthropogenic 

(such as possible oil-spill related) organic-matter content. 

Sediment samples for this project are analyzed for metals and other trace elements; organic 

compounds including PAH, SVOC, and Oil and Grease; benthic invertebrates; ambient 

populations of hydrocarbon-degrading microorganisms; and will undergo analysis of porewater 

toxicity as well as oil-fingerprinting analyses of tarball and bulk-sediment hydrocarbons. 

7.1 Objectives and Method Overview and Preparations

Samples should be collected in a manner such that they accurately represent ambient conditions 

at the time of sampling. The extent of apparent oil penetration into the nearshore beach (swash) 

sediments at sampling locations is to be determined and documented. Swash-zone sediments are 

subject to scouring, resuspension, and deposition from surf action; therefore, swash-zone 

samples are collected from an area and at a depth horizon to which oil might have penetrated. 

For the purpose of this study, wet sediment samples are collected at the land/water interface 

(swash zone) on beaches and from bottom materials of streams that dissect wetland areas. Swash 

and wetland sediments are collected in the exclusion zone (EZ, Section 4), a cordoned-off area 

large enough to allow two sets of benthic invertebrate samples (three samples per set) to be 

collected from about 0.5 to 1 m apart. Sediment coring, collection, and homogenization of a bulk 

(composite) sample follows the procedures described below and as required by site conditions at 

the time of sampling. 

1. Plan sampling with consideration of weather and tidal conditions, if possible. The 

variability of tidal range may affect the viability of sample locations at mid to high tides. 

In addition, sediments in the land/water interface may differ substantially at different 
64 

stages of tide. If possible, sample collection should be conducted at comparable tidal 

stages as those collected during the pre-impact sampling at a given location. 

2. Perform a general site survey prior to site entry, in accordance with the HASP (Section 4 

and Appendix E). 

3. Prepare dedicated sets of equipment for each site and as appropriate for the planned 

analysis (see Appendix D, Table D–2, for sediment sampling). This equipment will have 

been previously quality controlled by collecting and analyzing blank-water samples of 

the appropriate grade for a full suite of the same organic and inorganic constituents for 

which samples will be analyzed. 

a. Precleaned or certified-clean sample containers. WhirlPaks used for the bacteria 

samples must be certified and maintained as sterile.

b. Precleaned and quality-assured Teflon bags, for lining the bucket in which a bulk 

composite of sediment will be prepared. These are to be autoclaved and kept sterile in 

autoclaved bags for transport to the field. 

c. Polycarbonate and Teflon coring devices and Teflon scoops, spoons, and spatulas that 

have been certified or quality assured as clean of target analytes and wrapped to 

ensure they are kept clean and contanminant-free during packaging and transport to 

the field site. If used to collect the bacteria sample, these must be autoclaved prior to 

use. 

d. Precleaned, Teflon-bag-lined, 2.5-gallon bucket in which to composite a bulk 

sediment sample.

4. Install stakes or flagging and police-barrier tape to identify and mark the boundary of the 

sampling location (EZ) and CRZ. If necessary, the proposed sampling location may be 

adjusted based on site access, property boundaries, and surface obstructions. 

a. Record GPS data for the sampling locations (sample markers are temporary).

b. Document specific site and sediment characteristics, including the extent and 

description of any observed contaminant. 

c. Photograph the location and a profile of the trench or core at which samples are to be 

collected. Take site photos facing north, south, east, and west, close-ups, and a 

view looking directly down at the sediment-collection area. Photos should be dateand-time stamped and labeled with site ID and an arrow indicating the orientation and 

direction toward which the photo was taken. When photographing the core or trench 

profile, include a ruler or other marker to indicate scale and, if not obvious, which 

side is up. 

5. After sampling, scoops/spades/spoons/spatulas and core tubes either are disposable and 

appropriately discarded or, if designated for reuse, are to be cleaned of surface 

contamination in the CRZ and stored in ziplock bags for transport to the office laboratory 

where they will be cleaned using the chemical agents appropriate for the equipment type 

and degree of contamination, per routine USGS decontamination protocols. Rinsate 
65 

blanks may be collected periodically to verify the efficacy of the cleaning procedure for 

any equipment that will be reused. 

7.2 Equipment and Supplies

The intent of this protocol, as applied to the USGS response to the Deepwater Horizon oil spill, 

is to use quality-assured, precleaned sampling and single-use disposable equipment at each 

sampling site to the extent possible (table 4 and table 5). Precleaned Teflon equipment will be 

used primarily to collect and composite beach and wetland sediments. Any equipment that will 

be reused will be cleaned and quality assured as described in Section 4 of this report. 

Sample integrity is dependent on proper selection and use of sampling equipment, laboratory 

containers and preservatives, and the decontamination procedures use for cleaning of equipment 

that can contact the sample to be collected. The equipment and supplies selected for sample 

collection, processing, and handling shall meet the specifications of the analyses to be performed

(see table 4 below and the information provided in Appendix B). 
66 

Table 4. Containers and preservatives specific to sediment collection.

[BGC, baked glass container; CIN, laboratory’s analytical identification number; HEM, N-hexane extractable material; NFSS, USGS National 

Field Supplies Service; PAH, polycyclic aromatic hydrocarbons; SVOC, semivolatile organic compounds; TCL, target compound list; mL, 

milliliter; oz, ounce; L, liter]

Sample Container/

Chemical Preservative

Type of Analysis 

Laboratory

Container Source1

One 250- mL certified BGC. 

No preservative.

Tar ball degradation 

R. Rosenbauer, USGS, Menlo Park, Calif.

One Stop - NFSS

I-Chem or equivalent

Six 500-mL sterile plastic 

containers.

Three cores only preserved with 

10-percent sodium-borate 

buffered formalin.

Benthic invertebrates 

A. Demopoulos, USGS, Gainesville, Fla.

One Stop - NFSS

One 18-oz (532-mL) WhirlPak, 

sterile.

No preservative. 

Microoganisms

J. Lisle, USGS, St. Petersburg, Fla.

One Stop - NFSS

Two 1-L wide-mouth BGC. No 

preservative. 

Pore-water toxicity

R. Carr and J. Biedenbach, USGS, Corpus Christi, 

Tex.

One Stop - NFSS

Two 500-mL certified BGC. No 

preservative. 

Oil fingerprint

R. Rosenbauer, USGS, Menlo Park, Calif.

One Stop - NFSS 

I-Chem or equivalent

One 18-oz (532-mL) WhirlPak, 

beach sand; or,

Two 18-oz (532-mL) WhirlPak, 

fine-grained wetland sediments.

No preservative.

Trace metals and nutrients2

A. Horowitz, USGS, Norcross, Ga.

One Stop - NFSS 

One 8-oz wide-mouth glass 

container.

No preservative.

Oil & Grease (Method HEM, CIN 50137 )

SVOC TCL (Method – 8270, CIN 50117) 

TestAmerica, Pensacola, Fla. (TAL)

TAL - Pensacola

One 4-oz wide-mouth clear 

glass container. No 

preservative.

PAH and Alkylated PAH (Method 8270C, CIN 

50641)

TestAmerica, Pensacola, Fla. (TAL)

TAL - Pensacola

1 NFSS items are available as an oil-spill kit (Q613fld) prepared specifically for this project. 2 Analysis includes: Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Li, Mn, Hg, Mo, Ni, P, Se, Ag, Sr, Tl, Sn, U, V, Zn, Al, C 

(inorganic + organic), Organic C, Fe, N, S, Ti.

Note: Add the extra sample containers needed when the work schedule calls for the collection of quality-control 

samples.
67 

Table 5. Supplies for sediment sampling. 

[ASR-CoC, Analytical Services Request -Chain of Custody; cm, centimeter; gal, gallon; in, inch; mil, 1/1000th of an inch in thickness]

Supplies Specific to Sediment Sampling1

√ 3-gal Teflon bucket liners, cleaned

√ 2.5-gal plastic bucket 

√ Polycarbonate tube, 2.5-in (6.5 cm) inside diameter, 6 in (about 15 cm) long

√ 10-percent formalin solution saturated with sodium borate -- benthic invertebrate sample preservation 

√ Teflon core tubes, 1.5-in diameter by 12-in length 

√ Disposable or cleaned Teflon®, sampling scoops, plate; and spades or spatulas 

√ Plastic sheeting for homogenization and containerization area

√ Laboratory forceps, metal or Teflon

General Supplies

√ Barricade (police) tape for Exclusion and Contamination Reduction Zones

√ Digital camera

√ Tape measure

√ Survey stakes or flags

√ Nitrile gloves

√ Photo Ionization Detector (vapor analyzer)

√ Deionized water in spray bottle

√ Ziploc bags 4-mil gauge; leak-proof coolers

√ Wet Ice and Dry Ice, Trash bags, heavy duty

√ ASR-CoC and Field forms (Appendix F)

1

Refer to Appendix B for a completed list of sampling equipment and supplies. Refer to Section 7.5.1.1 for supplies for sediment 

quality-control sampling.
68 

7.3 Site Process and Order of Sample Collection

Sediment sampling occurs after water samples have been collected and appropriately packed in 

coolers. The third team member should begin immediately to facilitate sediment-sampling 

preparations as water sampling winds down. A synopsis of sampling requirements for each type 

of sample analysis is shown in figure 8 and summarized in Appendix D, table D–2. Go to 

Section 7.4 for the step-by-step procedures to be used for this project. 

7.3.1 Initial Site Process

After entering the EZ and before collecting sediment in the Teflon-lined bucket: 

Wearing nitrile gloves, remove any thick layer of product from the beach surface by blotting it 

with an absorbent cloth to expose sand surface. Change gloves.

• Remove large rocks, sticks, shells, and tar balls (greater than 2 mm). Change gloves.

• Collect a 9-in. core, using the PVC or a Teflon tube, following the procedures detailed in 

Section 7.4. This core is used only to document strata characteristics and the presence of 

visible oil; sediment from this core is not to be used for or combined with sample being 

prepared for laboratory analysis. 

With the exception of the samples for analysis of benthic invertebrates and tar balls, a bulk 

sample will be collected and homogenized in a 2.5-gallon Teflon-bag-lined bucket, from which 

subsamples will be collected for the rest of the sediment analyses. 

• Beach sediment. Samples of beach sediment are collected from the top 9 to 10 in. of the 

swash zone, using a Teflon core tube or Teflon scoop to fill a 2.5-gallon Teflon-lined 

bucket to about three-quarters capacity. 

• Wetland sediment. Wetland sediments are collected from the top 4 to 6 in. of submerged 

sediment, using a Teflon scoop to fill a 2.5-gallon Teflon-lined bucket to about threequarters capacity.

After collecting each sample: 

• Use a Kimwipe or cloth to clean the outside of the container. 

• When capping sample jars, wipe the container and lid threads free of sediment before 

sealing the container closed. This prevents possible leaks and loss of sample. Tape the lid 

as instructed by the analyzing laboratory.

• Referring to Appendix D, Table D–2: 

− Place the container into a foam or bubble sleeve and then into doubled ziplock bags. 

Seal the ziplock bags.

− Store all samples immediately on dry or wet ice, as specified by the analyzing 

laboratory. 

• Follow CoC instructions explicitly (refer to Section 8).
69 

7.3.2 Order of Sample Collection 

1. Tar balls – One 250-mL laboratory-certified glass jar. Chill.

2. Benthic invertebrates – Six 500-mL plastic jars – 1 core per jar; 3 cores equal one 

sample set. Preserve as directed. Chill.

3. Collect subsamples from the bulk sample:

a. Toxicity10 – Two 1-L wide-mouth glass jars. Chill, do not freeze. 

b. Microorganisms – One 18-oz (532 mL) Whirl-Pak. Freeze.

c. Oil Fingerprint – Two 500-mL wide-mouth jars, fired. Freeze.

d. Metals/Trace Elements and Nutrients – One 18-oz (532 mL) WhirlPak for beach 

sand; two 18-oz WhirlPaks for fine-grained (for example, wetland) sediments. Chill, 

do not freeze. 

e. PAH/Alkylated PAH – One 4-oz wide-mouth jar. Chill. 

f. Oil and Grease/SVOC/percent moisture – One 8-oz wide-mouth clear glass. Chill.

TAKE NOTE! Protect samples from contacting ice meltwater during transport: Seal the ice in 

doubled bags and place each sample into a separate doubled ziplock bag.

 

10 Toxicity analysis of pore water in the bulk sediment sample is dependent on maintaining good moisture content. 

The order in which the sample for toxicity analysis should be collected therefore depends on the professional 

judgment of the field team to ensure sufficient moisture content in this sample.
70 

Figure 8. Flowchart showing sediment sampling, Gulf of Mexico Deepwater Horizon oil spill, 2010.
71 

7.4 Step-By-Step Procedures

Deploy to the swash EZ if at a beach site (or to a boat if needed for site access) with the 

necessary equipment. Before preparing to sample swash-zone sediments in a beach environment, 

field personnel are to collect a 9-in (about 23 cm) to 10-in core to capture a depth profile, as 

follows (this step could be accomplished by digging a trench in lieu of collecting a core, field 

conditions permitting): 

1. Press a coring tube (PVC or Teflon) into the swash-zone sediments to collect a core of 9 

to 10 in from land surface. Dig around the tube to allow for sliding a spatula or Teflon 

plate across the tube bottom( to hold the sediment in the tube while the tube is extracted). 

2. Carefully extrude the core from the core tube onto a plastic sheet. Measure and describe 

distinct or mixed horizons and the pattern of any apparent oil infiltration; take detailed 

photographs of the core (be sure to include a measurement reference) and record 

observations in the logbook. Slice the core in half lengthwise and record observations. 

7.4.1 Tar-Ball Sample Collection

1. Tar-ball specimens should be thumbnail to palm size. These can be collected from 

anywhere at the beach or wetland site. Photograph each specimen in situ (before its 

removal).

2. Remove tar ball(s) using a Teflon scoop or metal forceps.

3. Place specimens in a 250-mL laboratory-certified clean glass jar (a 125-mL jar may be 

used, if available). 

4. Store and ship frozen to the USGS, Menlo Park, Calif., laboratory. 

5. Record a description of the collection location; for example, swash, low/mid/high tide, 

GPS coordinates. Photograph the collection area before and after collection.

7.4.2 Benthic Invertebrate Sample Collection 

Sampling for benthic invertebrates requires collection of two sets of samples (three separate 

cores per sample set) at each site, collected approximately 0.5 to 1 m apart in the EZ. To obtain 

the sample for benthic invertebrates, a 2.5-in (6.4-cm) inner diameter, 15-cm-long polycarbonate 

core tube is used to collect a core sample of the top 5 cm of the sediment profile. Each core is 

extruded into a separate container. Only one set of samples is preserved chemically. Both must 

be kept chilled. The specific steps for collecting these samples follow: 

1. Put on disposable nitrile gloves.

2. Remove the precleaned disposable coring device from the protective packaging.

3. Push the polycarbonate coring device exactly 2 in (5 cm) into the sediment (to the setmark on the side of the core tube).

4. Carefully slide a precleaned spatula (without slots) under the core tube to enclose the 

sample. Endeavor not to disturb the sediment inside the coring device.

5. Carefully remove excess sediment and any oil from the outside of the coring device with 

a clean Kimwipe. 
6. Extrude and gently tap the core into a 500-mL plastic jar.

7. Inspect the inside of the coring device and spatula surface and use forceps to remove and 

place any remaining organisms into the container. 

8. Repeat steps 3 through 7 five times to complete collection of two (three-core) sample

sets.

9. Sample set 1: To three of the jars that comprise one sample set, add 10-percent formalin 

supersaturated with sodium borate preservative. Cap each jar securely (after clearing jar 

and lid threads of sediment) and invert each jar several times to evenly disperse the 

preservative. 

10. Sample set 2: Do not add chemical preservative to the second (three-core) sample. 

Ensure that jar and lid threads are clear of sediment, and cap each securely. 

11. Wrap duct tape around the lids to seal each jar; wrap each jar in a Kimwipe or paper 

towel and place in doubled ziplock bags. 

12. Label the sample jars with the date and time – each offset by 2 minutes – and the name 

o

a.

f the collector and the site identifer. Record the collection of the sample in the logbook 

a

b.

nd on the ASR/CoC and field-notes forms

For Sample set 1, write "10% buffered formalin" on the label of each jar. 

For Sample set 2, write “unpreserved sa

.

mple” on the label of each jar. 

13. Place samples on ice to keep chilled at or below 4°C and ship overnight to the USGS, 

Gainsville, Fla., laborator

at 4°C, keep samples on dr

y). If there is any delay in shipping or keeping samples chilled 

y ice and place in a freezer upon return to the office; ship 

frozen the following day.

14. Replace outer pair of gloves with a clean pair in preparation for the next sample. 

7.4.3 Bulk Sample Collection

A bulk sample will be collected and homogenized as a composite and subsampled for chemical 

or microoganism analyses, as described below. Remember to use an absorbent cloth to blot up 

any oil that might be pooled on the surface of the sampling area. Teflon bucket liners (large 

Teflon bags) are used to line the bucket and contain the bulk sample and should be used in a 

manner to ensure that contact with the sample is restricted to the inside, quality controlled, and 

autoclaved portion of the liner. The liners are discarded after each use. The step-by-step 

procedures described below should be customized to fit the conditions experienced by the field 

team; however, any procedure used that deviates from this protocol is to be documented in detail 

in the logbook. Before beginning sample collection, review the project plan and site objectives 

and determine if replicate samples are required (see Section 7.5.2). Plan accordingly. To the 

degree possible, field teams should maintain consistent sampling procedures among all sites.

7.4.3.1 Collecting the Bulk Sample

Line a clean 2.5-gallon bucket with precleaned and sterile Teflon bags (doubled), wearing 

precleaned gloves and inserting the bag to ensure that the outside of the bag lines the bucket and 

the quality-controlled interior will contain the sediments. 

72 
73 

Beach site: 

1. Push a 30.5-cm (12-in) Teflon core tube vertically into the top 23 to 25.5 cm (9 to 10 in) 

of sediment. 

2. Dig around the perimeter so that a Teflon plate can be slipped under the bottom of the 

core and contain the water-laden sediments until the core can be emptied into the Teflonlined bucket. Since the toxicity analysis of the sediment porewater is to be performed for 

this project, take care to retain the water in the sample.

3. Repeat steps 1 and 2 above to fill the bucket. 

a. Using the Teflon scoop and avoiding contact with your gloved hand, homogenize the 

sample after emptying every one to two cores into the bucket. Take care to sample 

and homogenize in a manner that maintains the moisture content of the sample and 

minimzes evaporation. 

b. Continue until the bucket is filled to about three-quarters of capacity. 

c. Collect the sample for toxicity analysis. Toxicity analysis of pore water in the bulk 

sediment sample is dependent on maintaining good moisture content. The order in 

which the sample for toxicity analysis should be collected therefore depends on the 

professional judgment of the field team to ensure sufficient moisture content in this 

sample. Keep the bulk sample homogenized after removal of each subsample. 

Wetland site: 

1. Using a sterile Teflon scoop, collect the top 4 to 6 in. of wetted sediment so that the bulk 

sample represents the sampling area; empty the sediment into the bucket. 

2. Maintaining a wetted condition is critical when collecting sample for toxicity analysis, as 

it is the porewater that is extracted for the analysis. Since toxicity analysis is included in 

this project, decanting of excess water should be minimized. (For projects for which this 

is not a concern, decant excess water from the Teflon scoop carefully so as to avoid loss 

of fine sediments before emptying sediment into the bucket.) 

3. Using the Teflon scoop and avoiding contact with your gloved hand, homogenize the 

sample after emptying every two or three scoops into the bucket. 

4. Repeat steps 1 through 3 above until the bucket is about three-quarters full.

5. Collect the sample for toxicity analysis first or as appropriate to ensure that a high 

moisture content is retained in the sample 

7.4.3.2 Subsampling the Bulk Sample 

1. Move from the swash or wetland sampling area to a dry, plastic-lined area appropriate for 

sample containerization. 

a. If the sampling site was accessed by boat, the sampling team must determine how 

much of this phase of the sampling operation can be carried out on the boat 

(preferred), or if it must be carried out onshore. 

b. The sample should not be allowed to dry. 
74 

2. Wipe off the bucket before setting it down on top of clean plastic sheeting. Change 

gloves. 

3. Check if QC samples are to be collected and ask Sampler 3 to set up additional 

containers, if needed. 

4. Sampler 2: Hand the subsampling tool to Sampler 1 and uncap and hold the container for 

Sampler 1 to fill. 

5. Sampler 1: Remix the bulk sample thoroughly, so as to be completely homogenized. Mix 

for about 5 minutes, in a manner to prevent evaporation of the moisture content. 

6. Sampler 2: Select the tool for subsampling and the sample container, as appropriate for 

the sample analysis, and hand it to Sampler 1. Uncap and hold the container for Sampler 

1 to fill with sediment.

7. Sampler 1: Fill the sample container, leaving headspace as described below for the 

analysis of interest (refer also to Table D–2 in Appendix D). 

8. Sampler 2: Hand the container and cap to Sampler 3. 

9. Sampler 3: Remove any sediment, mud, or oily substance from the outside of the 

container, paying attention to the cap and container threads; secure the lid to the container 

by taping around the lid to seal it to the container. Wipe container dry; affix, fill out, and 

check label; place container in bubble or foam sleeve, double bag in ziplock, and put the 

sample into the appropriate shipping cooler. 

10. Samplers 1, 2 and 3: Continue steps 3 through 7 until all samples have been collected and 

stored on ice. Each analysis requires specific containers and volumes of sediment as 

described in the steps that follow. Fill all required sample containers with homogenized 

sample volumes as specified:

a. Toxicity in Pore water11

: Two 1-L wide-mouth clear glass jars. Fill jars with highmoisture content sediment, to bottom of threads. Seal lids with electrical tape. Chill 

samples at or below 4°C; do not freeze. 

b. Microoganisms: Using sterile equipment, fill an 18-oz. (532 mL) Whirl-Pak and seal 

in another WhirlPak. Freeze sample. 

c. Oil Fingerprint: Two 500-mL amber glass, lab-certified wide-mouth jars. Fill jars 

to about 80 percent of capacity; keep jars upright. Freeze samples on dry ice.

d. Metals/Trace Elements and Nutrients (TP, TN, TS): Collect about 1 kg for sandsized sample into two 18-oz. (532 mL) WhirlPak bags; collect about 500 g for mud 

and fine-grained sediments into one 18-oz. (532 mL) WhirlPak. Seal each sample in 

another WhirlPak. Chill, do not freeze. 

e. SVOC TCL: One 8-oz wide-mouth TAL glass jar. Fill jar, tape lid. Chill.

f. PAH /Alkylated PAH: One 4-oz wide-mouth TAL jar. Fill jar,tape lid. Chill.

g. Oil and Grease: One 8-oz fired wide-mouth TAL jar. Fill jar, tape lid. Chill.

 

11 The sample for toxicity analysis requires high moisture (porewater) content. Professional judgment of field 

personnel should be used to determine whether, given existing field conditions, this requirement is best achieved by 

collecting the toxicity subsample first or last.
75 

7.4.4 Wrap-Up Procedures

1. Record the collection of sample in the field logbook. Multiple ASR field forms are 

needed to manage the CoC in individual coolers to the appropriate laboratory. Examples 

of the ASR/CoC forms needed for each laboratory are in Appendix F. Refer to Table D–2 

in Appendix D for a list of laboratory addresses and contacts, and container and shipping 

requirements. 

2. Return excess soil from the composite (bulk) container to the point of collection. Rinse 

sediment and debris from the bucket. 

3. Deploying to the CRZ, remove and discard all disposable PPE, used Teflon bags and 

other sampling gear, the ground sheeting, and decontamination liquid and solid materials 

into designated and properly labeled receptacles. 

4. Complete the decontamination process as described in Section 4.0. If site access was by 

boat, complete as much of the decontamination process as possible on board. 

7.5 Collection of Quality-Control Samples

The samples to be collected for quality control of sediment collection include equipment blanks 

and replicates, as described below. Be careful to use the correct ASR forms that are designated 

for QC samples and that indicate the applicable QC method code. If more than one replicate 

sample is included, distinguish between replicates with time steps. Consult Table 2 of Appendix 

D for preservation and shipping requirements. 

7.5.1 Equipment Blanks

Blank samples (rinsate blanks) will be collected for quality assurance of the sediment collection 

and processing equipment. The bucket liner, sediment scoop, and core tube and plate are rinsed

with IBW and VPBW for inorganic and organic analyses, respectively. The rinsate is collected in 

the containers used for water samples. Detection of analytes targeted for this project in the 

rinsate water is considered a sensitive indication of possible contamination from the equipment 

to the environmental sediment sample. 

7.5.1.1 Supplies for equipment blanks

• Two (2) Teflon bucket liners (disposable)

• Teflon scoop(s), Teflon plate, and Teflon core tube 

• Nitrile gloves

• 2.5-gal plastic bucket

• Inorganic Blank Water (IBW) (estimate three bottles)

• Organic Blank Water (VPBW) (estimate four 12-L bottles)

• 250-mL HNO3-preserved bottle from TAL 

• 250-mL H2SO4-preserved bottle from TAL 

• 18-oz (532-mL) Whirlpak and 500-mL glass jar to contain water-filled Whirlpak
76 

• Four (4) VOA vials from TAL, 2 for VOCs and 2 for TPH GRO 

• 8-oz wide-mouth glass jar from TAL for Oil-and-Grease analyses

• 4-oz clear glass jar from TAL for PAH/Alkylated PAH 

• 250-mL glass jar from NWQL for oil-fingerprint analysis 

• Two (2) 1-L glass jars from NWQL for toxicity analysis

• 1-L Teflon bottle for surfactant analysis*

• 125-mL bottle for DOC analysis*

• Cleaning solutions and solution-treatment and disposal materials: Refer to NFM 3.

* For these analyses, research scientists have requested blank samples of sediment equipment for 

surfactant and DOC analyses, in addition to those representing equipment used for collection of 

water samples.

7.5.1.2 Collection of Equipment Blanks for Sediment-Sampling Equipment 

Follow standard USGS protocols and procedures (NFM chapter 3) for cleaning the Teflon 

equipment for sediment sampling listed above, with the following modification for precleaning 

the Teflon scoop, core tube, and core plate: Replace the 5-percent HCl-solution rinse with a 10-

percent by volume bleach-solution rinse; thoroughly remove the bleach residue from this 

equipment with multiple rinses with sterile IBW or VPBW (see Section 4). 

Leave sufficient headspace when filling sample containers to allow for expansion of the chilled 

samples. Equipment-blank samples should not be frozen. 

To collect sediment-equipment rinsate blanks: 

1. Put on nitrile gloves; be prepared to change gloves with each change in procedure. 

2. Line the bucket with a cleaned, sterile Teflon liner. 

3. Prepare to collect VPBW for rinsate samples for organic analyses. Place a Teflon 

rectangle (core plate), scoop, tube, and another bucket liner into the lined bucket. 

4. Open a fresh bottle of VPBW and use about 1-liter of VPBW to rinse your gloves, the 

extra liner, and each piece of Teflon equipment. Place the loose equipment into the extra 

liner (keeping it in the lined bucket), discard the water in the bucket, and repeat the 

VPBW rinse on each piece of equipment two more times. 

5. Transfer the Teflon equipment from the liner to the lined bucket. Use the extra liner as a 

clean surface on or in which to place the scoop. 

6. Pour about 6 liters of VPBW into the lined bucket. Using clean-hands/dirty-hands 

techniques (NFM chapter 4) and the Teflon scoop, fill the following sample containers, 

refilling the bucket with VPBW as needed: 

• 18-oz Whirlpak in glass jar — Microorganisms 

• 8-oz glass amber — Oil & Grease 

• 4-oz clear glass — PAH/Alkylated PAH 

• Two 500-mL glass jars — Oil Fingerprinting 

• Two 1-L glass jars — Toxicity 
77 

• 1-L Teflon bottle — Surfactant/dispersant (DOSS)

• 125-mL DOC glass bottle – Dissolved organic carbon 

7. Empty the equipment and VPBW from the bucket, placing equipment in clean, protected 

environment. 

8. Open a fresh bottle of IBW. Rinse gloves, bucket, Teflon bucket liner, and all the Teflon 

equipment three times with IBW. 

9. Place liner and all the Teflon equipment except the scoop and second liner back in the 

bucket and fill with IBW. Place the Teflon scoop on or in the extra rinsed Teflon bucket 

liner. 

10. Using clean-hands/dirty-hands techniques, fill the sample containers using the Teflon 

scoop, as follows: 

• 250-mL preserved polyethylene bottle for metals/trace elements 

• 250-mL preserved bottle for nutrients 

7.5.2 Replicate Samples

As a rule of thumb, collect at least twice as much material as is required for sites at which 

replicates will be collected. Homogenize the material and containerize as described below into 

two individual sample containers. Label each container with its unique sample, site, and (or) 

station identifier and record the original and duplicate as separate samples on the CoC/ASR. 

• Duplicates – for TAL ananlysis only. Collect one set of duplicates, per WSC, per site 

type (beach and wetland).

− Oil & Grease and SVOC analyses: Collect one sample in addition to the first 

environmental sample in an 8-oz wide-mouth jar. 

− Alkylated PAH/PAH: Collect one sample in addition to the first environmental 

sample in a 4-oz wide-mouth jar. 

• Triplicates – for TAL and each research laboratory. Triplicates are collected only at

oiled sites. Collect one set of triplicates, per WSC, and for only one site type (beach or 

wetland), as follows: 

− Oil and Grease and SVOC analyses: Collect two samples in addition to the first 

environmental sample in 8-oz wide-mouth jars. 

− Alkylated PAH/PAH: Collect one additional sample in a 4-oz wide-mouth jar. 

• Benthic Invertebrates: Collect an additional 12 cores, each extruded into a 

500-mL plastic jar. Preserve six of the cores with buffered formalin. 

• Oil Fingerprint: Collect additional bulk sediment samples into four 500-mL fired 

glass wide-mouth jar. 

• Trace Elements and Nutrients: Collect additional bulk samples by filling two 

18-oz (532-mL) Whirlpaks for fine-grained material; if the sediment is coarse 

grained, fill four additional 18-oz (532-mL) Whirlpak samples. 
78 

• Microorganisms: Collect additional bulk samples by filling two 18-oz (532-mL) 

Whirlpaks. 

• Pore-water toxicity: Collect additional bulk samples by filling four 1-L widemouth glass jars. 
79 

8.0 Chain of Custody and Documentation Requirements: Labeling, 

Packaging, and Shipping

8.1 Method Summary

Samples collected for the post-landfall oil spill require legally defensible data. The following 

protocols for field documentation, sample labeling, packaging, and shipping incorporate the use 

of standard chain-of-custody (CoC) procedure as applied to environmental samples. The 

instructions and procedures provided in this section comprise a summary of Standard Operating 

Procedure for Chain of Custody Samples, Office of Environmental Measurement and 

Evaluation, USEPA New England - Region 1 (U.S. Environmental Protection Agency, 2002a). 

However, the exact chain-of-custody requirements to be implemented can depend also on the 

unique characteristics of a specific operation; field teams should verify CoC protocols with their 

Unified Command and other administrative contacts before the start of field work. 

8.2 Field Procedures

Field personnel are legally responsible for the care and custody of the samples collected until the 

samples are transferred to a laboratory or otherwise properly dispatched.

• As few people as possible should handle the samples. 

• Each sample container must be labeled, at a minimum, with a station number and 

identifier, date and time of collection, and sampler’s name. 

• Sample labels are to be completed for each sample using indelible ink (such as nonerasable black or blue “rite-in-the-rain” ballpoint pen). If weather conditions prohibit use 

of a ballpoint pen and a pencil is used instead, this must be noted in the field logbook. 

Sharpies® or other similar pens that emit fumes are prohibited from use. 

8.2.1 Field Logbooks and Other Documentation 

The field logbook (logbook) will provide a means for recording field observations and the datacollection activities performed. Logbooks are to be bound, paginated field survey books or 

notebooks, preferably with “rite in the rain” properties. 

Logbook entries should be as detailed as needed so that personnel going to the site at a later date 

can reconstruct a particular situation without reliance on memory. 

• At the beginning of each day, record the date, start time, weather, names of all sampling 

team members present, level of personal protection being used, and the signature of the 

person making the entry. Assign a temporary site ID if a station ID has not been 

established for the sampling site.

• Include a record of the names of visitors to the site and additional field-sampling or 

investigative personnel, and the purpose of the visit. 

• Record measurements made and samples collected, along with a detailed description of 

the location of data collection. 
80 

• All entries will be made in ink as described above, and no erasures will be made. If an 

incorrect entry is made, the information will be crossed out with a single strike mark and 

the entry will be initialed and dated. 

• Logbook entries and field record sheets must include site and station identifier (ID), date, 

time, and names or initials of all persons handling the sample in the field.

Field forms have been customized for this project (Appendix F) and can be used to supplement 

logbook entries, although their use will not substitute for recording the major onsite activities 

and data entries according to CoC protocol. The equipment used to collect samples will be noted 

on these field forms, along with the time of sampling, sample description/purpose, depth at 

which the sample was collected, sample volume, and number of containers and samplepreservation procedures. Duplicate field samples receive separate and unique site identifiers (ID) 

if the corresponding station IDs have not yet been set up; sample, site, and (or) station ID 

numbers are recorded field forms. Equipment used to determine field-measurement data are

identified by make, model, and serial or unique ID number along with the date and time of 

calibration or calibration checks. 

Photographs are to be taken from multiple perspectives (north, northwest, south, etc.) to 

document the general condition and characteristics of the field site and of the specific location of 

sample collection. If possible, photographs should be stamped with the GPS coordinate 

information for both field-site and sample-collection location

8.2.2 Labeling Sample Containers 

Sample labels shall be completed for each sample collected for analysis, using waterproof ink, as 

described above. If working under the jurisdiction of the Natural Resource Damage Assessment 

and Restoration Program, labeling conventions and sample nomenclature may differ from those 

routinely used within the USGS; ensure that correct nomenclature protocols are in place. Figure 

9 provides an example of a sample label. The information to be recorded on the sample tag or 

label includes:

• Site and Station ID numbers. 

• Date: A six-digit number indicating the year, month, day of collection. 

• Time: A four-digit number indicating the local standard or daylight time datum (EST, 

EDT, CST, CDT) time of collection using the military or 24-hour time convention; for 

example, 0954. 

• Station Name (descriptive). 

• Site Description. 

• Name of personnel collecting and handling the sample(s) (provide full name). 

• Parameter (analyte) and sample preservation: the sample analysis to be conducted and 

how the sample is preserved using physical and/or chemical means. 

• Comments: Pertinent observations of any site conditions that might affect the quality of 

the analysis.
81 

 Site ID:_______________ Station ID:______________ 

 Lab:__________________ Station Name: __________ 

Sample Type:___________ Project No:_____________ 

Media:_________________ 

 Analysis:_____________________________________________ 

Preservative:__________________ 

 

 Location:_________________________________________________________ 

 

Sample Date:_________________ Sample Time:_________________ 

 Sample ID: __________________ Depth:_______________________ 

Sampled By:______________________________________________________ 

 

Comments/Site Description:_________________________________________ 

 _________________________________________________________________ 

 _________________________________________________________________ 

Figure 9. Example of a sample label.

Due to the evidentiary nature of samples collected during environmental investigations, 

possession of the sample must be traceable from the time the samples are collected until they are 

introduced as evidence in legal proceedings. This chain of custody (CoC) will be documented 

using the Analytical Services Request (ASR) form to inform the laboratory of the analyses being 

requested for each sample and to document sample possession and custody. One signed copy of 

the ASR form should remain with the sampler and two copies should be transported with the 

sample aliquots to each laboratory. 

It is the intent of this protocol to follow USEPA policy regarding sample custody and CoC 

protocols, as described in Sample Custody—NEIC Policies and Procedures, EPA-330/9-78-

DDI-R, revised June 1985. This custody procedure is in three parts: sample collection, laboratory 

analysis, and final evidence files. Final evidence files, including originals of laboratory reports 

and electronic files, are maintained under document control in a secure area. A sample or 

evidence file is under your custody when: 

• It is in your possession, or 

• It is in your view, after being in your possession, or 

• It was in your possession and then locked up to prevent tampering, or 

• It is in a designated and documented secure area.
82 

To maintain a record of sample collection, a CoC/ASR record will be completed for each sample 

destined for laboratory analysis and for the transfer of samples among sample custodians, 

shipping courier, and the laboratory. Examples of standard CoC/ASR forms for water and 

sediment samples that are shipped to TestAmerica Laboratory, Pensacola, Fla., are provided in 

Appendix F. 

Sample CoC/ASR procedures require that the possession and handling of the sample from the 

moment of its collection through analysis be documented by written record. The record must 

clearly reflect the movement of the sample through the CoC/ASR to ensure the sample has been 

positively controlled and has not been tampered with in any way. Each time the samples are 

transferred, the signatures of the person relinquishing and receiving the samples, as well as the 

date and time of transfer, will be documented. 

8.2.3 Transfer of Custody and Sample Shipment 

Samples are to be properly packaged for shipment (see Appendix D) and dispatched to the 

appropriate laboratory for analysis. Samples must be accompanied by a properly completed 

CoC/ASR form at all times.

• The CoC/ASR form is signed and dated with the time of transfer by a member of the 

field team who has verified that those samples indicated on the CoC/ASR form are indeed 

being shipped. 

• The station name, ID, and locations are listed on the CoC/ASR form. 

• A separate signed custody record is enclosed in each sample box or cooler. 

After packaging is complete, the shipping containers are secured with strapping tape and custody 

seals for shipment to the laboratory. The custody seals must be signed and dated either by a 

member of the field team or by those designated and certified by the Unified Command, 

and placed over the lid edge for fixed-base laboratory samples. The preferred procedure also 

includes using a custody seal attached to the front right and back left of the cooler. Ensure that 

strapping tape does not cover and hide the CoC tape. 

All samples are shipped by an appropriate courier (for example, Federal Express). Samples are 

transported daily or the next day from the sampling or storage location to the courier location for 

subsequent shipment to the laboratory. If the courier will not sign the CoC form, this should be 

noted on the form with the time of transmittal to the courier. A designated member of the field 

team should track the time of shipment and progress to its destination until its arrival is 

confirmed by the laboratory. Upon receipt of the samples at the laboratory, the receiver will 

complete the transfer by dating and signing the CoC/ASR form. If shipped by commercial 

courier, the air bill number and shipping data will be transcribed to the CoC/ASR form in the 

appropriate signature/date block. A copy of the air bill is to be kept with the field copy of the 

CoC/ASR form to reflect specific shipping information.

The custodian of the evidence file will maintain the contents of evidence files for each 

investigation, including all relevant records, reports, logs, field notebooks, pictures, 

subcontractor reports, correspondence, laboratory logbooks, and CoC forms. 
83 

• Each project evidence file will be stored in a secure, limited-access area and under 

custody. A copy of the CoC/ASR shall be kept by the sample team. 

• Analytical laboratories will retain all original CoC documents and raw analytical data 

information (both hard copy and electronic) in a secure, limited-access area and under 

custody of the laboratory-designated project manager.

• Sample collection points, station identification numbers, and sampling dates documented 

in the field logbooks will be verified with the information written on the sample label and 

(or) CoC/ASR form.

8.2.3.1 Packaging Samples

Equipment and material requirements to properly handle, ship, and maintain custody of samples 

as described in the preceding sections include the following: 

• Teflon, duct, and electrical tape for sealing lids on sample containers and vials 

(as directed by the receiving laboratory) 

• Chain-of-Custody forms

• Properly labeled sample containers 

• Indelible black ink marker

• Custody seals, moisture-proof; can adhere to wet coolers 

• Approved, non-leaking and undamaged coolers of various sizes with drains sealed

• Temperature check sample

• Ziplock bags (assorted sizes for samples and ice)

• Plastic trash bags

• Bubble wrap or foam sleeves

• Ice – wet and dry

• Courier airbills

• Laboratory contact information 

• Nylon reinforced strapping tape

• Any special requirement courier labels (hazardous materials, caustic, etc.)

• Lockable storage areas (to maintain sample custody, may be locked vehicle, office, etc.)

• Coolers for shipping samples: clean, leak-proof. To avoid loss of shipping labels from 

“sweating” coolers, it is recommended that the sender and recipient address be written in 

indelible marker on the outside of the cooler. 

Lids or caps on sample containers are to be taped with Teflon, electrical, or duct tape, when so 

directed by the receiving laboratory to help prevent leakage. Glass containers will be wrapped 

with plastic insulating material (such as foam or bubble wrap) to prevent contact with other 

sample containers or the inner walls of the cooler; containers also are to be sealed in doubled 

ziplock bags. Similar containers for the same location may be sealed in the same set of ziplock 

bags (for example, VOC and TPH-GRO vials).
84 

Sample identification from each container shall be compared to the entries on the CoC/ASR form 

to ensure bottle labels and CoC entries match. Once this is confirmed, the samples can be packed 

as described. Wet ice is required to be bagged in doubled bags and sealed to prevent leakage 

from melting ice. 

Samples will be packaged in thermally insulated, rigid coolers, according to DOT specifications 

(173 Subparts A and B and 172 Subparts B, C, and D). Environmental samples and field qualitycontrol blanks to be submitted to the analytical laboratory will be placed in a shipping cooler 

along with ice and temperature blanks. After a cooler is filled, the appropriate CoC/ASR form 

will be placed inside a resealable plastic bag and taped to the inside lid of the cooler, and the 

outer surface of the cooler will be cleaned. Any leaking cooler will be held by the courier and 

sample holding times could be missed.

TAKE NOTE! The bubble or foam wrap on glass sample containers might prevent the sample 

from being appropriately chilled or frozen. Sufficient ice must be in contact with the wrapped 

container to ensure thermal preservation of the sample.

The cooler shall be secured with CoC tape and custody seals, followed by using a minimum of 

three complete wraps of nylon-reinforced strapping tape on each end of the cooler and to help 

secure, but not hide, the CoC tape and seals. Signed custody seals must be applied, at a 

minimum, at the front and back of the cooler such that the seal would be broken if the top is 

opened or removed. An example of a custody seal is shown in figure 10. 

Figure 10. Example of a custody seal.

8.2.3.2 Shipping Samples

Whenever possible, ship samples to the laboratory overnight on the day of collection. Pay strict 

attention to holding-time limitations for the given sample type; for example, the holding time of 

the VOC and TPH samples, collected in VOA vials, is 7 days from collection to analysis. Check 

laboratory hours of operation—keep in mind that the laboratory might not receive samples on 

Saturdays, Sundays, or holidays. The integrity of chilled samples sent late on a Thursday or on a 

Friday could be compromised if not received by the laboratory in time to be unpacked and 

refrigerated.

• Check the planned arrival time before selecting the courier service.
85 

• Courier services will not accept or deliver leaky boxes or coolers. Securely tape the 

outside of shipping coolers to help prevent leaking. 

• Do not exceed maximum weight and size restrictions set by the courier service.

• Comply with the courier service’s requirements for meeting U.S. Department of 

Transportation regulations for transporting hazardous substances. 

− Identify any samples that require special shipping procedures (for example, samples 

to be shipped on dry ice). 

− Send chilled and frozen samples to the laboratory by the fastest means possible.

− Obtain instructions and authorization from the laboratory before sending any highly 

contaminated or potentially hazardous samples to the laboratory for analysis. 

• Shipping of sediment samples for this project must conform to Federal regulations and 

procedures. Do not ship sediment samples in coolers containing samples of water, tissue, 

or media other than sediments. 

TAKE NOTE! Avoid overfilling the shipping coolers. Packing the coolers too tightly can cause 

breakage of the cooler and its contents, especially when containing frozen samples and dry ice.
86 

9.0 Quality Assurance and Quality Control for Field Sampling

The purpose of this section is to address the topic of quality assurance (QA) as it applies in 

general to USGS sampling efforts in response to the Deepwater Horizon oil spill and to describe 

the actions and protocols to be implemented for quality-control (QC) samples collected after 

landfall of the oil spill. The standard operating procedures referred to in this section follow those 

given in the National Field Manual for the Collection of Water-Quality Data (U.S. Geological 

Survey, variously dated) and may need to be modified according to circumstances encountered in 

the field or because of changes or redefinition of data-quality objectives for the sampling effort. 

The rationale for deviation from this protocol must be documented in field logbooks at the time 

of sampling. 

9.1 Quality-Assurance Requirements

The USGS defines quality assurance (QA) as those procedures used to control the 

nonquantifiable components of a project, including the development and use of this sampling 

protocol. Examples of key components of QA for this project and for water-quality projects in 

general that are required to fulfill the objectives of this project are listed below. 

• Standard, scientifically valid and appropriate methods and protocols for the collection of 

in situ environmental field measurements and water and sediment data are used and 

documented. Data must be produced in such a manner so as to ensure that site conditions 

are represented accurately at a time and location that fulfill project and data-quality 

objectives. 

• Adherence to strict protocols is critical for documenting site conditions and field activities, 

including implementation of those requirements for maintaining a legal record of chain of 

custody for all samples that are collected; for example, properly entering data in bound, 

paginated, project-dedicated logbooks and on field data sheets and laboratory request 

forms. 

• Equipment that contacts the sample must be constructed of materials that cannot itself 

become a source of sample contamination. In other words, the equipment used must not be 

capable of releasing measurable concentrations of the same analytes that are targeted for 

study. In this regard, it is recommended that all sample containers be quality assured and, 

when appropriate, carry certification of laboratory-grade cleanliness. 

• Equipment cleaning and decontamination procedures are required that have been tested 

and are known to be appropriate and effective for work in crude-oil-contaminated land and 

aqueous environments. 

− Protocols for removal of the cleaning and decontamination agents used on equipment 

must be followed strictly so the cleaning process itself does not become a source of 

contamination to the sample. For example, methanol must be allowed to evaporate 

completely from all equipment surfaces, nooks, and crannies; only nonphosphate 

detergents will be used, and subsequently these and any acid solutions must be rinsed 

thoroughly from all equipment surfaces. 
87 

− Standard hazardous-waste handling and disposal procedures (described in Section 4), 

involve the proper containment and disposal of contaminated materials, including the 

waste fluids and materials from equipment decontamination. Such procedures are 

meant to ensure that cross contamination of samples does not occur among and 

between sites and that contamination is not transferred offsite to public or private 

areas.

• Disposable equipment that has been precleaned and quality assured will be used, where 

and when possible, in order to prevent the possibility of cross-contamination between 

sampling sites and to minimize the need for onsite equipment decontamination by use of 

organic solvents and acids. 

• Field personnel are aware of those routine procedures that might affect the ambient 

environment in which samples are collected. For example,

− When boats are used, boat motors and bilge pumps should be turned off during the 

sampling operation and retrieval and decontamination of sampling equipment, to 

avoid creating an additional and not ambient source of contamination. 

− Storage—permanent and transient—of gasoline or other petroleum-based products 

and methanol and methanol-infused rags or clothing must be kept in a secure area that 

is separate and downwind of the sample-collection, sample-processing/preservation, 

and packaging areas. 

• Collection and analysis of QC samples, such as blank, replicate (samples collected in 

duplicate, triplicate, etc.), and spike samples, whose purpose it is to assess the quality of 

environmental data by generating a set of data that will be used to estimate the magnitude 

of the bias and variability resulting from the procedures used for obtaining the samples. 

− For blank samples, laboratory-certified blank water of the appropriate grade is

obtained, stored, transported, and used in accordance with standard USGS 

procedures: Inorganic-grade blank water (IBW) for metals/trace-element and nutrient 

analyses and nitrogen gas-purged volatile/pesticide-grade blank water (VPBW) for 

each of the organic-compound analyses.

− Matrix spikes, prepared at the laboratory by laboratory personnel. 

• Mandated training for all field personnel to ensure that health and safety regulations and 

sampling and data-collection methods are understood and appropriately implemented. 

9.2 Summary of Quality-Control Sampling for the USGS Response to the Deepwater 

Horizon Oil Spill

Quality-control samples are to be collected and analyzed along with environmental samples to 

assist in identifying the occurrence, source, and magnitude of sample contamination (field and 

laboratory) and as a measure of variability in the analytical composition of samples collected. 
88 

Analysis of the unimpaired sediments collected during the pre-landfall phase of this project will 

serve as a baseline against which to compare analytical results from the post-landfall samples. 

In order to provide useful information, QC samples must be collected, prepared, and analyzed in 

the same manner and using the same materials as were used for environmental samples. Failure 

to do so is likely to result in invalid or indeterminate interpretations of the QC data and can 

compromise the scientific defensibility of the data. 

9.2.1 Frequency and Distribution

Quality control for the coastal samples will rely primarily on the collection of replicate and 

specified types of blank samples at a frequency of not less than one (1) in 10 samples by each 

Water Science Center, or as otherwise prescribed in Sections 6.5 and 7.5 for the QC sample type. 

Additional (extra) QC samples should be collected according to the best professional judgment 

of the field team leader as needed to account for the bias and variability of unanticipated site 

conditions; for example: (1) the potential for cross contamination of the samples from the 

environment may be much greater at sites with a more visible presence of oil, alerting the 

sampler to the need to collect a precautionary blank sample; (2) a PID scan may signal 

heightened concern for bias to VOC samples, resulting in collection of an ambient-condition 

blank (ambient field blank). 

The specific sites at which various types of QC samples are collected and the frequency of 

visiting these sites is to be determined by USGS Water Science Center team leaders after the 

start of post-landfall sampling. 

9.2.2 Quality-Control Sample Types 

Quality-control samples for specified water and sediment analyses as described in Section 6.5 

and Section 7.5, respectively, will be collected by each USGS Water Science Center (WSC). 

• Blank samples:

− One set of equipment blanks before deploying to the field. For sediment equipment, 

rinsate blanks will be collected by using and subsequently analyzing laboratorycertified blank water in which sediment equipment has been immersed. 

− One set of ambient field blanks will be collected for water analyses by the 

TestAmerica Laboratory (TAL), Pensacola, Fla., to determine the potential for sample 

contamination from ambient (environmental) field conditions occurring during the 

time of sample exposure to the atmosphere. 

− TAL provides trip blanks for quality control of VOC and TPH-GRO water analyses

to determine if the integrity of these samples was comprised as a result of the sampletransport process. 

− Temperature blanks are included in each sample cooler and checked by the receiving 

laboratory to ensure that sample-preservation requirements with respect to 

temperature have been met.
89 

• Replicate and matrix-spike samples: 

− Duplicate samples: One set each of water and sediment samples are to be collected 

by each Water Science Center at one beach and one wetland site, and will be sent to 

TAL, Pensacola, to be analyzed only for those analyses for which TAL has been 

contracted. Duplicates are not to be collected for the research laboratories unless 

specifically requested.

− Triplicate samples: One set each of water and sediment samples are to be collected 

at one site with visible oil-related contamination, selected by the Water Science 

Center, and sent to each research laboratory and TAL for a full suite of analyses. 

• Laboratory matrix-spike samples: Water samples are to be collected at one Centerselected site at which no oil-related contamination is evident. The sample is fortified 

(spiked) at TAL and analyzed for semivolatile organic compounds (SVOCs) and dieselrange total petroleum hydrocarbons TPH-DRO).

In summary: 

• Water Samples (Section 6.5) 

− Equipment blanks – for analyses by TAL and selected Research labs 

− Ambient field blanks –1 site per WSC – TAL analyses only. 

− Trip blanks – provided by TAL, for VOC and GRO coolers 

− Temperature Blanks – provided by TAL, all coolers 

− Duplicates –1 site per WSC, per site type (beach or marsh) –TAL analyses only 

− Triplicates –1 oiled site per WSC –TAL and Research Lab analyses

− Matrix spikes –1 clean site per WSC, per site type –TAL (SVOC, TPH-DRO

analyses) 

• Sediment Samples (Section 7.5) 

− Equipment (rinsate) blanks – water for analyses by TAL & selected Research labs

− Duplicates –1 site per WSC, per site type (beach, wetland) –TAL analyses only 

− Triplicates –1 oiled site per WSC –TAL and Research Lab analyses

− Temperature Blanks – provided by TAL, all coolers 

9.3 Definitions and Description of Typical Quality-Control Sample Types

The information that follows provides a general overview of quality-control sample types, some 

of which may not relate directly to the work outlined for this project. 

9.3.1 Field Replicates

Field replicates are used to assess the variability associated with sample heterogeneity, sample 

methodology, and analytical procedures. Two or more field samples are obtained from one 

location, either concurrently or sequentially (one after the other). Following collection, they are 
90 

treated as separate samples throughout the remaining sample handling and analytical processes.

• Split Replicates consist of a composite or homogenized sample that is split into equal 

volumes using appropriate, quality-assured methods, and placed into the appropriate 

containers. (For this project, no water samples will be prepared as split replicates.) 

• Sequential Replicates consist of samples collected separately but close in time (one after 

another). Spatial distance among sequential replicates can depend on the media and the 

intended analysis. 

− For sediment to be analyzed for VOCs, for example, it is advised that distinct and 

nonhomogenized samples be collected from 1 to 3 feet apart. (For this project, 

sediment samples will not be collected for VOC analysis.) 

− For water sampling, sequential replicates are collected as close in time and space as 

possible. (For this project, sequential replicates will be collected for water samples 

only.) 

− Each container is assigned a unique sample identifier, and labeled and recorded on the 

CoC/ASR form as separate samples. 

9.3.2 Matrix Spikes

Matrix-spike samples are used to evaluate interference from the environmental matrix on the 

performance of the analytical method. A replicate set of sample containers are collected for 

sediment and/or water and identified as spike samples for each analysis for which a matrix spike 

is to be requested. The sample generally is fortified with the spiking solution in the laboratory. 

Each container is assigned a unique identifier, and each is labeled and recorded on the CoC/ASR 

as separate samples. (For this project, sediment samples will not be collected for matrix-spike 

analysis.) 

9.3.3 Field Blanks 

A field blank is a category of QC sample that is prepared in the field to assess cross 

contamination caused (a) by inadequate decontamination procedures or contamination of a 

sample from a source not associated with the sample matrix, such as sampling equipment or 

sample-handling and transport procedures, or (b) ambient atmospheric conditions at the time of 

sampling (ambient blank). Since samples for this project are collected primarily using 

precleaned, dedicated, disposable equipment few, if any, field blanks will be collected. Blank 

samples, therefore, will focus on collection of ambient field blanks to determine the potential for 

sample contamination from ambient field conditions occurring during the time of sample 

exposure to the atmosphere. 

• Field blanks generally are collected at a rate of one (1) in every 10 to 20 samples for a 

given analyte, or at a greater frequency, depending on ambient field conditions or 

decontamination-related requirements and project approach and objectives. 

• Ambient field blanks are to be collected before collecting environmental samples while at 

the sampling location. For this project, ambient field blanks will be collected for VOCs

when organic-vapor concentrations exceed 15 ppmv (determined by PID scan). 
91 

• A rinsate blank may be collected to test the suitability of reused equipment after it has 

been decontaminated. Decontamination of equipment to be reused can be accomplished 

either on site or in the office laboratory, according to the best judgment of field personnel 

(Section 4.0 of this protocol). All equipment must be rinsed and appropriately 

containerized before being transported from the field site. 

9.3.4 Equipment Blanks 

Equipment blanks are required to test the suitability of new, disposable (single-use) equipment as 

well as reusable equipment. Equipment blanks are collected in the office or laboratory to ensure 

a clean and controlled sampling environment that is protected from ambient (such as airborne) 

contaminants. A one-time equipment blank per type of equipment is collected by each Water 

Science Center before sampling begins (see Sections 6.5 and 7.5 for collection of water and 

sediment equipment blanks, respectively.) This protocol does not apply to laboratory-supplied 

sample containers that are certified clean for the chemical constituents of interest.

Equipment blanks (in some cases these are the same as rinsate blanks) are obtained by collecting 

blank water of the appropriate type from or through sampling equipment after having gone 

through an established cleaning procedure (refer to NFM chapter 3 in U.S. Geological Survey, 

variously dated) and before its first use in the field. The purpose of the equipment blank is to 

ensure that the equipment itself and the prescribed equipment-cleaning or decontamination

procedures are not potential sources of contamination to the samples that the equipment will 

contact. 

Equipment blanks are collected well before project field work begins to allow time for these 

samples to be analyzed by their respective laboratories and for the results to be evaluated. Should 

laboratory results indicate the presence of a constituent or compound that is targeted for study, 

the Water Science Center team first should consult with other Centers engaged in this project to 

determine if similar problems have been found. The field team is accountable to review their 

cleaning and sampling procedures, how the equipment was handled and stored, repeat the 

cleaning and blanking procedure for each piece of equipment separately, and review analytical 

results for the new set of equipment-blank samples until they are satisfied that they understand 

and have solved the problem. The protocols and procedures related to collection of equipment 

blanks for this project are the same as those used routinely for USGS water-quality projects and 

as documented in chapter 4, section 4.3 of the National Field Manual (see U.S. Geological 

Survey, variously dated). 

9.3.5 Source-Solution, Temperature, and Trip Blanks

• A source-solution blank may be collected for VOC analysis to document if the 

composition of the blank water, as received and stored before transport to the field, was 

free of measurable concentrations of the VOCs to be analyzed. 

• Temperature blanks will ensure that sample-preservation requirements with respect to 

temperature have been met.

• Trip blanks for VOC analyses are collected to determine if the integrity of these samples 

could have been comprised by the sample-transport process. 
92 

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Aiken, G.R., McKnight, D.M., Thorn, K.A., and Thurman, E.M., 1992, Isolation of hydrophilic 

acids from water using macroporous resins: Organic Geochemistry, v. 18, p. 567–573. 

Alonso-Gutierrez, J., Costa, M.M., and others, 2008, Alcanivorax strain detected among the 

cultured bacterial community from sediments affected by the Prestige oil spill: Marine Ecology 

Progress Series 362, p. 25–36. 

Carr, R.S., 1998, Sediment porewater testing, in section 8080 of Standard Methods for the 

Examination of Water and Wastewater (20th ed.):Washington, D.C., American Public Health 

Association, p. 8–37 to 8–41. 

Carr, R.S., and Biedenbach, J.M., 1999, Use of power analysis to develop detectable significance 

criteria for sea urchin porewater toxicity tests: Aquatic Ecosystem Health and Management, v. 

2, p. 413–418. 

Carr, R.S., Montagna, P.A., Biedenbach, J.M., Kalke, R., Kennicutt, M.C., Hooten, R., and 

Cripe, G., 2000, Impact of storm water outfalls on sediment quality in Corpus Christi Bay, 

Texas: Environmental Toxicology and Chemistry, v. 19, p. 561–574. 

Crone, T.J. and Tolstoy, M., 2010, Magnitude of the 2010 Gulf of Mexico oil leak: Science, v. 

330, p. 634 and online at http://www.sciencemag.org/content/early/2010/09/23/ 

science.1195840.abstract, accessed March 28, 2011. 

Demopoulous, A.W.J., Cormier, N., Ewel, K., and Fry, B., 2008, Use of multiple chemical 

tracers to define habitat use of Indo-Pacific mangrove crab, Scylla serrata (Decapoda: 

Portunidae): Estuaries and Coasts, v. 31, p. 371–381. 

Demopoulos, A.W.J., Fry, B., and Smith, C.R., 2007, Food-web structure in exotic and native 

mangroves—A Hawaii-Puerto Rico comparison: Oecologia, v. 153, p. 675–686. 

Demopoulos, A.W.J., and Smith, C.R., 2010, Invasive mangroves alter macrofaunal community 

structure and facilitate opportunistic exotics: Marine Ecology Progress Series, v. 404, p. 51–

67. 

Demopoulos, A.W.J., Smith, C.R., and Tyler, P.A., 2003, Ecology of the deep Indian Ocean 

floor, in Tyler, P.A., ed., Ecosystems of the world volume 28—Ecosystems of the deep ocean: 

Amsterdam, Elsevier, 569 p. 

Eganhouse, R.P., 1982, Organic matter in municipal wastes and storm runoff—Characterization 

and budget to the coastal waters of southern California: Ph.D. thesis, University of California. 
93 

Eganhouse, R.P., and Kaplan, I.R., 1982, Extractable organic matter in municipal wastewaters—

1. Petroleum hydrocarbons - Temporal variations and mass emission rates: Environmental 

Science and Technology, v. 16, p. 180–186. 

Eganhouse, R.P., and Kaplan, I.R., 1982, Extractable organic matter in municipal wastewaters—

2. Hydrocarbons - molecular characterization: Environmental Science and Technology, v. 16, 

p. 541–551. 

Eganhouse, R.P., and Pontolillo, James, 2008, Assessment of 1-chloro-4-[2,2-dichloro-1-(4-

chlorophenyl)ethenyl]benzene (DDE) transformation rates on the Palos Verdes Shelf, CA: 

U.S. Geological Survey Open-File Report 2007–1362, 114 p. 

Eganhouse, R.P., Dorsey, T.F., Phinney, C.P., and Westcott, A.W., 1996, Processes affecting the 

fate of monoaromatic hydrocarbons in an aquifer contaminated by crude oil: Environmental 

Science and Technology, v. 30, p. 3304–3312. 

Eganhouse, R.P., Simoneit, B.R.T., and Kaplan, I.R., 1981, Extractable organic matter in urban 

stormwater runoff.—2. Molecular characterization: Environmental Science and Technology, 

v. 15, p. 315–326. 

Ferrer, I., Schroder, H., and Furlong, E., 2003, Atmospheric pressure ionization mass 

spectrometry – IX, LC-MS analysis of cationic surfactants—Methods and applications, in

Knepper, T., Barcello, D., and De Voogt, P., Analysis and fate of surfactants in the aquatic 

environment: Elsevier, p. 353–383. 

Fishman, M.J., and Friedman, L.C., eds., 1989, Methods for determination of inorganic 

substances in water and fluvial sediments: U.S. Geological Survey Techniques of WaterResources Investigations, book 5, chap. A1, 545 p. 

Frysinger, G.S., Gaines, R.B., Xu, L., and Reddy, C.M., 2003, Resolving the unresolved 

complex mixture in petroleum-contaminated sediments: Environmental Science and 

Technology, v. 37, p. 1653–1662. 

Furlong, E., Ferrer, I., Gates, P., Cahill, J., and Thurman, M., 2003, Identification of labile polar 

organic contaminants by atmospheric-pressure tandem mass spectrometry, in Ferrer, I., and 

Thurman, M., eds., Liquid chromatography/mass spectrometry, MS/MS and time of flight MS: 

ACS Symposium Series 850, p. 175–187. 

Gaines, R.B., Frysinger, G.S., Hendrick-Smith, M.S., and Stuart, J.D., 1999, Oil spill source 

identification by comprehensive two-dimensional gas chromatography: Environmental Science 

and Technology, v. 33, p. 2106–2112. 

Gertler, C., Gerdts, G., Timmis, K.N., and Golyshin, P.N., 2009, Microbial consortia in 

mesocosm bioremediation trial using oil sorbents, slow-release fertilizer and bioaugmentation: 

FEMS Microbiology Ecology, v. 69, p. 288–300. 
94 

Horowitz, A.J., Elrick, K.A., and Smith, J.J., 2001, Estimating suspended sediment and trace 

element fluxes in large river basins—Methodological considerations as applied to the 

NASQAN programme: Hydrological Processes, v. 15, p. 1107–1132. 

Kvenvolden, K.A., Hostettler, F.D., Rosenbauer, R.J., Lorenson, T.D., Castle, W.T., and 

Sugarman, S., 2002, Hydrocarbons in recent sediment of the Monterey Bay National Marine 

Sanctuary: Marine Geology, v. 181, p. 101–113. 

Lorenson, T.D., Hostettler, F.D., and others, 2009, Natural offshore oil seepage and related 

tarball accumulation on the California coastline—Santa Barbars Channel and the Southern 

Santa Maria Basin; source identification and inventory: U.S. Geological Survey Open-File 

Report 2009–1225, 116 p. 

MacNaughton, S., Stephen, J.R., Venosa, A.D., Davis, G.A., Chang, Y-J., and White, D.C., 

1999, Microbial population changes during bioremediation of an experimental oil spill: 

Applied and Environmental Microbiology, v. 65, p. 3566–3574. 

Moulton, S.R., II, Kennen, J.G., Goldstein, R.M., and Hambrook, J.A., 2002, Revised protocols 

for sampling algal, invertebrate, and fish communities as part of the National Water-Quality 

Assessment Program: U.S. Geological Survey Open-File Report 02–150, 75 p. (Also available 

at http://pubs.usgs.gov/of/2002/ofr-02-150/index.html.) 

Murphy, K.R., Butler, K.D., Spencer, R.G.M., Stedmon, C.A., Boehme, J.R., and Aiken, G.R., 

2010, The measurement of dissolved organic matter fluorescence in aquatic environments—

An interlaboratory comparison: Environmental Science and Technology, v. 44, p. 9405–9412. 

National Oceanic and Atmospheric Administration, 2007, Heat index calculator: National 

Oceanic and Atmospheric Administration, accessed August 19, 2010, at 

http://www.hpc.ncep.noaa.gov/html/heatindex.shtml. 

Natural Resource Damage Assessment and Restoration Program, 2010, Protocols for collecting 

NRDA samples: U.S. Department of the Interior Natural Resource Damage Assessment and 

Restoration Program, National Resource Damage Assessment Guidance, May 11, 2010. 

Occupational Safety and Health Administration (OSHA), 2010, Deepwater Horizon/Mississippi 

Canyon 252 oil spill, OSHA Fact Sheet.

Occupational Safety and Health Administration (OSHA), 2010, Safety and health awareness for 

oil spill cleanup workers, OSHA Oil Spill Cleanup Initiative, v.4, May 2010. 

Reddy, C.M., Eglinton, T.I., Hounshell, Aubrey, White, H.K., Xu, Li, Gaines, R.B., and 

Frysinger, G.S., 2002, The West Falmouth oil spill after thirty years—The persistence of 

petroleum hydrocarbons in marsh sediments: Environmental Science and Technology, v. 36, p. 

4754–4760. 

Roling, W., Milner, M.G., and others, 2004, Bacterial community dynamics and hydrocarbon 

degradation during a field-scale evaluation of bioremediation on a mudflat beach contaminated 

with buried oil: Applied and Environmental Microbiology, v. 70, p. 2603–2613. 
95 

Rosenbauer, R.J., Campbell, P.L., Lam, Angela, Lorenson, T.D., Hostettler, F.D., Thomas, Burt, 

and Wong, F.L., 2010, Reconnaissance of Macondo-1 well oil in sediment and tarballs from 

the northern Gulf of Mexico shoreline, Texas to Florida: U.S. Geological Survey Open-File 

Report 2010-1290, available online only at http://pubs.usgs.gov/of/2010/1290/. 

Rosenbauer, R.J., Campbell, P.L., Lam, Angela, Lorenson, T.D., Hostettler, F.D., Thomas, Burt, 

and Wong, F.L., 2011, Petroleum hydrocarbons in sediment from the northern Gulf of Mexico 

shoreline, Texas to Florida: U.S. Geological Survey Open-File Report 2011-1014, 22 p.

3M Corporation, 2010, Personal protective equipment for oil spill response: 3M Corporation 

Occupational Health and Environmental Safety Division, Technical Data Bulletin #195, May 

2010. 

U.S. Environmental Protection Agency, 1985, Sample custody—NEIC policies and Procedures: 

EPA 330-9-78-DDI-R, Revised June 1985. 

U.S. Environmental Protection Agency, 1994, US EPA contract laboratory program national 

functional guidelines for inorganic data review: EPA 540-R-94-013, February 1994. 

U.S. Environmental Protection Agency, 1996, Marine toxicity identification evaluation (TIE)—

Phase I guidance document: EPA 600/R-96/054. 

U.S. Environmental Protection Agency, New England-Region 1, 1998, Draft calibration of field 

instruments: U.S. Environmental Protection Agency, June 3, 1998. 

U.S. Environmental Protection Agency, 1999, US EPA contract laboratory program national 

functional guidelines for organic data review: EPA 540-R-99-008, February 1999. 

U.S. Environmental Protection Agency, California - Region 9, 1999a, Field sampling guidance 

document for sediment sampling: U.S. Environmental Protection Agency Richmond 

Laboratory, September 1999. 

U.S. Environmental Protection Agency, California - Region 9, 1999b, Field sampling guidance 

document for trace metal clean sampling of natural waters: U.S. Environmental Protection 

Agency Richmond Laboratory, September 1999. 

U.S. Environmental Protection Agency, New England - Region 1, 2002a, Standard operating 

procedure for chain of custody of samples: U.S. Environmental Protection Agency, Office of 

Environmental Measurement and Evaluation, March 25, 2002. 

U.S. Environmental Protection Agency, New England - Region 1, 2002b, Standard operating 

procedure for the collection of chemical and biological ambient water samples: U.S. 

Environmental Protection Agency, Office of Environmental Measurement and Evaluation, July 

24, 2002. 

U.S. Environmental Protection Agency, New England - Region 1, 2002c, Standard operating 

procedure for sample login, tracking and disposal: U.S. Environmental Protection Agency, 

Office of Environmental Measurement and Evaluation, July 26, 2002. 
96 

U.S. Environmental Protection Agency, New England - Region 1, 2004, Standard operating 

procedure for document control: U.S. Environmental Protection Agency, Office of 

Environmental Measurement and Evaluation, February 18, 2004. 

U.S. Environmental Protection Agency, Region 4, 2010a, Gulf Coast water quality monitoring 

quality assurance plan, Mississippi/Alabama/Florida: U.S. Environmental Protection Agency, 

Science and Ecosystems Support Division, May 1, 2010. 

U.S. Environmental Protection Agency, 2010b, Quality assurance sampling plan for British 

Petroleum oil spill: U.S. Environmental Protection Agency, May, accessed August 19, 2010, at 

http://www.epa.gov/bpspill/bp-oil-spill-sampling-plan.pdf. 

U.S. Geological Survey, variously dated, National field manual for the collection of waterquality data: U.S. Geological Survey Techniques of Water-Resources Investigations, book 9, 

chaps. A1–A9, available online at http://pubs.water.usgs.gov/twri9A. 

Chapters cited in this report are: 

Wilde, F.D., 2005, Preparations for water sampling: U.S. Geological Survey Techniques of 

Water-Resources Investigations, book 9, chap. A1 [http://pubs.water.usgs.gov/twri9A1/].

Lane, S.L., Flanagan, Sarah, and Wilde, F.D., 2003, Selection of equipment for water 

sampling: U.S. Geological Survey Techniques of Water-Resources Investigations, book 9, 

chap. A2 [http://pubs.water.usgs.gov/twri9A2/].

Wilde, F.D., ed., 2004, Cleaning of equipment for water sampling: U.S. Geological Survey 

Techniques of Water-Resources Investigations, book 9, chap. A3 

[http://pubs.water.usgs.gov/twri9A3/].

U.S. Geological Survey, 2006, Collection of water samples: U.S. Geological Survey 

Techniques of Water-Resources Investigations, book 9, chap. A4 

[http://pubs.water.usgs.gov/twri9A4/].

Wilde, F.D., Radtke, D.B., Gibs, Jacob, and Iwatsubo, R.T., eds., 2004 with updates through 

2009, Processing of water samples: U.S. Geological Survey Techniques of Water-Resources 

Investigations, book 9, chap. A5 [http://pubs.water.usgs.gov/twri9A5].

Wilde, F.D., ed., chapter sections variously dated, Field measurements: U.S. Geological 

Survey Techniques of Water-Resources Investigations, book 9, chap. A6 

[http://pubs.water.usgs.gov/twri9A6/].

U.S. Geological Survey, variously dated, Biological indicators: U.S. Geological Survey 

Techniques of Water-Resources Investigations, book 9, chap. A7 

[http://pubs.water.usgs.gov/twri9A7/].

Radtke, D.B., Revised 2005, Bottom-material samples: U.S. Geological Survey Techniques 

of Water-Resources Investigations, book 9, chap. A8 [http://pubs.water.usgs.gov/twri9A8/].
97 

Lane, S.L., and Fay, R.G., 1997, Safety in field activities: U.S. Geological Survey 

Techniques of Water-Resources Investigations, book 9, chap. A9 

[http://pubs.water.usgs.gov/twri9A9/]. 

Wagner, R.J., Mattraw, H.C., Ritz, G.F., Smith, B.A., 2000, guidelines and standard procedures 

for continuous water-quality monitors—site selection, field operation, calibration, record 

computation, and reporting: U.S. Geological Survey Water-Resources Investigations Report 

2000–4252, 53 p. (Also available at http://pubs.usgs.gov/tm/2006/tm1D3/.) 

Weishaar, J.L., Aiken, G.R., Bergamaschi, B.A., Fram, M.S., Fujii, R., and Mopper, K., 2003, 

Evaluation of specific ultraviolet absorbance as an indicator of the chemical composition and 

reactivity of dissolved organic carbon: Environmental Science and Technology, v. 37, p. 4702–

4708. 

Wilde, F.D., Skrobialowski, S.C., and Hart, J.S., 2010, Sampling protocol for post-landfall 

Deepwater Horizon oil release, Gulf of Mexico, 2010: U.S. Geological Survey Open-File 

Report 2010-1191, 83 p. with appendices. 
98 

11.0 Acronyms, Abbreviations, and Chemical Symbols

Ag Silver

Al Aluminum 

As Arsenic

ASR Analytical Services Request

ASTM ASTM International. (An organization for standardization of technical scientific 

and industrial methods) 

atm Atmospheric unit 

B Boron 

Ba Barium

Be Beryllium

BGC Baked glass container

BP British Petroleum Global Company

BTEX Benzene, toluene, ethylbenzene, and xylenes

C Carbon 

Cd Cadmium 

CDT Central Daylight Time

CFR Code of Federal Regulations

Co Cobalt 

CO2 Carbon dioxide 

CoC Chain of custody 

CPR Cardiopulmonary Resuscitation 

Cr Chromium 

CRC Contamination Reduction Corridor 

CRZ Contamination Reduction Zone 

CST Central Standard Time

Cu Copper 

Decon Decontamination

DI water Distilled/Deionized Water

DNA Deoxyribonucleic acid

DO Dissolved oxygen 

DOC Dissolve Organic Carbon 

DOI Department of the Interior 

DOSS Di(Ethylhexyl) Sodium Sulfosuccinate 

DOT Department of Transportation 

DRO Diesel-range organics
99 

DWH Deepwater Horizon

EDT Eastern Daylight Time

EST Eastern Standard Time

EZ Exclusion zone or Hot zone 

Fe Iron

FWS U.S. Fish and Wildlife Service

GOM Gulf of Mexico

GPS Global Positioning System 

GRO Gasoline-range organics

HASP Health and Safety Plan

HazWOper Hazardous Waste Operations and Emergency Response 

HCl: Hydrochloric acid

HF/HClO4 Hydrofluoric acid/perchloric acid 

Hg Mercury

HI Heat Index

HNO3 Nitric acid

H2SO4 Sulfuric acid

IBW Inorganic-grade blank water 

IC Incident Command 

ID Identifier

JHA Job Hazards Analysis 

LEL Lower Explosive Limit 

Li Lithium

MeOH Methanol 

mil 1/1000th of an inch in thickness 

Mn Manganese

Mo Molybdenum 

MOCC Motorboat Operator Certification Course 

MS/MSD Matrix-spike samples

MSDS Material Safety Data Sheet
100 

N Nitrogen

N Normal (normality of a chemical reagent)

NFM National Field Manual for the Collection of Water-Quality Data (U.S. Geological 

Survey Techniques of Water-Resourses Investigations, book 9, section A) 

NFSS National Field Supply Services of the USGS National Water-Quality Laboratory

NH4 Ammonium 

Ni Nickel

NIST National Institute of Standards and Technology 

nm Nanometer

NMR Nuclear magnetic resonance

NOAA National Oceanic and Atmospheric Administration

NWQL National Water Quality Laboratory (USGS)

O&G Oil and Grease

ORP Oxidation-reduction potential 

OSHA Occupational Safety and Health Administration

OWQ Office of Water Quality (USGS)

P Phosphorus 

PAHs Polycyclic Aromatic Hydrocarbons

Pb Lead

PEL Permissible Exposure Limit

PFD Personal Flotation Device 

PID photoionization detector 

PPE Personal Protective Equipment 

ppm: parts per million

ppmv parts per million by volume 

PVC Polyvinyl Chloride 

QA Quality assurance

QC Quality control 

QW Quality of water

RA Raw, acid-rinsed (sample container) 

ROX Reliable Oxygen Sensor (YSI Company) 

S Sulfur 

Sb Antimony

SC Specific Electrical Conductance

Se Selenium
101 

SI International System of Units (Système international d'unités)

SMIS Safety Management Information System

Sn Tin

Sr Strontium 

SVOC Semivolatile organic compounds 

SZ Support Zone (sometimes referred to as a safety zone)

TAL TestAmerica Laboratory

TC Total carbon

TCL Total carbon loss 

Ti Titanium

TIC Total inorganic carbon 

TKN Total Kjeldahl Nitrogen

Tl Thallium

TN Total nitrogen

TOC Total organic carbon 

TP Total Phosphorus 

TPH Total Petroleum Hydrocarbons 

TS Total sulfur 

U Uranium 

UEL Upper Explosive Limit 

UC Unified Command 

USCG U.S. Coast Guard 

USDA U.S. Department of Agriculture 

USEPA U.S. Environmental Protection Agency 

USGS U.S. Geological Survey

V Vanadium 

VOC Volatile Organic Compounds 

VOA Volatile organic analysis (vials for VOCs)

VOO Vessels of Opportunity 

VPBW VOC- and Pesticide-grade Blank Water (laboratory certified)

WSC Water Science Center of the U.S. Geological Survey 

Zn Zinc
102 

Appendix A. Collection of Baseline Samples in Response to the 

Deepwater Horizon Oil Spill and Location of Pre- and Post-Landfall 

Sampling Sites 

Appendix A–1. Plan for Collection of Baseline Water and Sediment Samples: 

Response to the Deepwater Horizon Oil Rig Explosion, Gulf of 

Mexico, April 2010, by the Texas, Louisiana, Mississippi, Alabama, 

and Florida Water Science Centers of the U.S. Geological Survey 

 

Appendix A–2. Pre- and Post-Landfall Sample Analyses and Laboratory Methods

Appendix A–3. USGS Gulf of Mexico Pre-Landfall and Post-Landfall Sampling Sites, 

2010 Oil Spill 

Appendix A–4. Maps Showing Locations of USGS Sampling Sites
103 

Appendix A–1. Plan for Collection of Baseline Water and Sediment Samples: 

Response to the Deepwater Horizon Oil Rig Explosion, Gulf of Mexico, April 2010, by 

the Texas, Louisiana, Mississippi, Alabama, and Florida Water Science Centers of the 

U.S. Geological Survey 

 

Contents Background

Objective and General Approach 

Data Collection 

Documentation

Quality Assurance and Quality Control

In Situ Water-Quality Measurements

Water Samples

Sediment Samples

Bulk Sediment Samples

Benthic Invertebrate Samples

Shipping and Chain of Custody

Table A–1. Sample analyses and laboratories for baseline data collection. 
104 

Background 

In response to the April 20, 2010, oil and natural gas explosion at the British Petroleum (BP) 

Deepwater Horizon oil rig and the subsequent oil spillage into the northern Gulf of Mexico, U.S. 

Geological Survey (USGS) Water Science Centers in Texas, Louisiana, Mississippi, Alabama, 

and Florida began coordinating efforts to collect samples from State and Department of the 

Interior lands that could experience severe environmental damage as a result of oil from this spill 

coming ashore. This document describes the USGS plan and protocol for collecting sediment and 

water samples from coastal beaches, wetlands, and barrier islands for the purpose of 

characterizing baseline chemical conditions and assessing other environmental indicators. A 

sediment sample at each site will be collected for anlaysis of benthic invertebrates. Sample 

collection will be coordinated through USGS Regional Executive Area Offices (South Central 

Area, Southeast Area) and the USGS Office of Water Quality. 

Objective and General Approach

The overall objective is to collect sediment and water samples before oil from the Deepwater 

Horizon spill arrives on shore (pre-landfall samples) and to analyze the samples to provide a 

baseline characterization of current chemical and specific biological conditions in those priority 

areas of the northern Gulf of Mexico that are at highest risk for oil contamination. Historic oil 

that is present will be identified by analyzing oil “fingerprints” and by examining results of 

analyses for polycyclic aromatic hydrocarbons (PAHs), oil and grease, trace metals, volatile 

organic compounds, surfactants, dissolved organic carbon, and benthic invertebrates (table A–1). 

In addition, bacterial populations capable of digesting oils and nutrients will be identified. 

Sediment and water will be collected from typical Gulf of Mexico environments, ranging from 

coastal wetlands to barrier islands and coastal sand beaches. All the samples will be collected at 

or near the land/water interface, as described below. Suitable sampling sites include wetlands, 

barrier islands, and shoreline beaches that can be sampled before oil from the Deepwater 

Horizon spill reaches them (that is, pre-landfall of the oil). No samples are to be collected from 

revetment sites or areas where treated pilings are present.

The methods to be used for collecting field data will follow the protocols described in the USGS 

National Field Manual for the Collection of Water-Quality Data (U.S. Geological Survey, 

variously dated; http://pubs.water.usgs.gov/twri9A), which includes standard procedures to 

prevent sample contamination (chapter 4, section 4.0, 9/2006) and procedures for use, cleaning, 

and storage and maintenance of the equipment and supplies used to carry out this field work 

(chapter 3). These methods are mandated to prevent or identify potential sources of sample 

contamination. A minimum of 2 weeks of training and experience in the use of these standard 

USGS protocols and procedures is required for all personnel participating in this data-collection 

effort.

Data Collection

The data to be collected include field observations; measurements of in situ water properties; and 

water, sediment, and invertebrate samples. Sample handling and shipping procedures will be in 

strict compliance with chain-of-custody requirements.
• Sample analysis and laboratories. The sample analyses and the laboratories at which the 

analyses will be performed are listed in table A–1. Brief descriptions of the laboratory and 

research methods used for sample analysis are compiled in Appendix C of this report. 

• Safety. All field and laboratory personnel should follow safety guidelines provided by 

their Water Science Center that relate specifically to this sampling effort, in addition to the 

standard protocols described in chapter 9 of the National Field Manual (U.S. Geological 

Survey, variously dated; http://water.usgs.gov/owq/FieldManual/Chap9/content.html). 

Field personnel should be aware that, by wearing the appropriate gloves for the sample 

collection, they will be protecting themselves from possible exposure to flesh-eating 

bacteria whose presence has been documented in the coastal areas of the Gulf of Mexico. 

Furthermore, personnel are advised to use antibacterial soap if their skin is compromised 

by cuts or scratches during the collection of samples.

Documentation

Site location, onsite observations, measurements of field properties, and the procedures used in 

the collection and preservation of water, sediment, and benthic invertebrate samples will be 

documented on field forms and in field notes. Data must be entered into the USGS National 

Water Information System (NWIS) and other databases that might be prescribed—data entry is 

to be timely, accurate, and quality assured. The procedures listed below are required, in addition 

to those described in chapter 4 of the National Field Manual at http://water.usgs.gov/owq/ 

FieldManual/chapter4/pdf/Chap4_v2.pdf, section 4.1, 9/2006 (see U.S. Geological Survey, 

variously dated: 

• The field team will use a Wide Area Augmentation System (WAAS) enabled GPS unit to 

record the location of each sampling site. 

• Field notes are to include comments regarding weather, wind speed, wave height, apparent 

health of vegetation, any organisms present and their conditions, the presence of possible 

contamination, water color, observed sediment grain size (sand, silt, clay, etc.), and the 

amount of organic detritus present at the site.

• Photographs will be taken at all sites as follows: the first photograph will be taken facing 

north 0o, then east 90o, then south 180o, and then west 270o. 

Quality Assurance and Quality Control

Onsite and equipment preparations, sample collection and preservation, and physical 

measurements of water quality will be conducted according to protocols described in the USGS 

National Field Manual. Samples of sediment and samples of water will be collected in triplicate 

and one field blank (water) will be collected at 10 percent of the sites for each of the USGS 

Water Science Centers on the Gulf of Mexico. The field blank is essentially a bottle blank, 

because no sampling equipment other than the sample bottle will be used for collecting water 

samples. 

105 
106 

In Situ Water-Quality Measurements 

Dissolved oxygen concentrations, pH, specific electrical conductance/salinity, and water 

temperature will be measured in situ at each site using a calibrated multiparameter data sonde; 

methods described in chapter 6 of the National Field Manual at http://water.usgs.gov/owq/ 

FieldManual/Chapter6/Ch6_contents.html (U.S. Geological Survey, variously dated) will be 

implemented. All calibration data (including adjustments and calibration checks) for the 

multiparameter instruments used to determine field measurements must be recorded in field 

notes and in meter logbooks. Final in situ measurements will be recorded on official field and 

analytical services request forms.

Water Samples

Water samples will be analyzed for selected inorganic and organic compounds, including 

di(ethylhexyl) sodium sulfosuccinate (DOSS) (a primary component of the Corexit surfactant 

used to disperse oil released by the Deepwater Horizon explosion). All water samples will be 

collected near the land/water interface using the “direct dip” sampling method. Sample bottles 

will be dipped at the water’s surface so as to give an accurate representation of any oil present at 

the site and in water deep enough to avoid resuspension of bottom material during sample 

collection. Each sample for a designated analysis will be collected and preserved in bottles of the 

type described in chapter 5 of the National Field Manual at http://water.usgs.gov/owq/ 

FieldManual/chapter5/html/Ch5_contents.html (U.S. Geological Survey, variously dated) or by 

the laboratory performing the analysis. Bottles used for the collection of samples for analysis of 

oil and grease should not be field rinsed before obtaining the sample to prevent 

overrepresentation of oil in the sample. All water samples will be accurately labeled, 

appropriately preserved with the prescribed chemical treatments, placed in an ice cooler, and 

chilled to maintain a temperature at or below 4oC (without freezing) until the samples have been 

received at the designated laboratory. The 125-mL sample for dissolved organic carbon (DOC) 

analysis will be collected as a wholewater sample and kept chilled at 4oC until it is filtered at the 

designated laboratory. 

Sediment Samples

Sediment samples must be packaged and shipped separately from water samples (see “Shipping 

and Chain of Custody”). 

Bulk Sediment Samples 

Sediment samples to be analyzed for microorganisms, toxicity, oil fingerprints, oil and grease, 

and selected inorganic and organic chemical components (table A–1) will be collected from a 

bulk sample. The bulk sample will be collected at the land/water interface (also called the swash 

zone) from the surface of the bed to a depth of 4 to 6 inches (in) using either a precleaned Teflon 

scoop or a grab sampler. A sufficient volume of sediment will be homogenized in a clean, white 

or uncolored plastic dish pan. The Teflon scoop will be used to mix the bulk sediment sample to 

form a well-mixed composite, which then will be split into the appropriate, labeled, sample 

containers. 
107 

• Subsamples for bacterial analyses (one sample from the swash zone and one from dry 

beach sand, if available) will be placed either in a 400-milliliter (mL) Whirl-Pak® bag or 

an appropriately sized resealable storage bag. 

• Subsamples for major- and trace-element and nutrient analyses will be placed in doubled 

ziplock bags. 

• Subsamples for toxicity, oil-and-grease, and oil-fingerprint analyses will be collected in 

fired glass containers, as stipulated on table A–1. 

All samples will be stored in an ice chest and kept at 4oC until shipped to the appropriate 

laboratory for analysis. 

Benthic Invertebrate Samples 

At each site, a single sediment core will be collected in the swash zone for taxonomic analysis of 

benthic invertebrates. To collect the sample, a coring tube (approximately 3-in or 7.6-centimeter 

(cm) diameter PVC pipe or plastic tube) is inserted vertically into the swash-zone substrate to a 

depth of 5 cm (2 in). Once the 5-cm depth is reached, the core sample is kept contained by 

carefully sliding a spatula (without slots) under the bottom of the coring tube. Care must be taken 

not to disturb the sediment inside the coring tube. Any sediment on the outside of the core tube 

must be carefully removed before extruding the sample into a resealable bag. Before sealing the 

sample bag, (a) the inside of the coring tube and spatula surface is inspected for any remaining 

organisms and the organisms are to be removed with a forceps and placed into the bag, and (b) as 

much air as possible should be expelled from the bag. The sample bags need to be chilled on ice 

until they can be placed in a sample freezer upon return to the office. Each sample bag must be 

labeled with the sampling date, name of the collector, and sampling location. 

USGS Water Science Center personnel are to make the coring tool either from a 3-in.-diameter 

PVC pipe or plastic sample bottle, as follows. (A similar application of this device is described in 

Moulton and others, 2002.) 

• PVC pipe as coring tube: Cut a PVC pipe to an appropriate length for ease of handling 

(for example, 4 or 6 in.). To facilitate insertion of the PVC pipe into the substrate, bevel 

the outer edge of the pipe. Carefully measure and mark the 2-in (5-cm) sampling depth on 

the inside of the pipe using a waterproof black marker. 

• Sample bottle as coring tube: Cut the bottom off of a 3-in.-diameter plastic sample 

bottle. The bottle should have a relatively flat bottom and must be cut evenly so as to 

retain a 5-cm-high side of the bottle. Drill a small hole in the center of the bottom; this 

will allow air to escape when the device is inserted into the sediment. When using this 

device, vertically insert the device into the sand (with the bottom side up) until the bottom 

is flush with the substrate. Carefully slide a spatula under the device to hold the sample in 

this core device until the sample can be extruded into a sealable plastic bag. 
108 

Shipping and Chain of Custody

Analytical services request (ASR) forms and chain of custody (CoC) forms appropriate for the 

laboratory to which samples are shipped must be filled out completely and signed per 

requirements. Each Water Science Center must use its user code to track data and charges; for 

example, Louisiana must designate user code LA and Texas must designate user code TX.

All samples will be shipped using CoC requirements and the appropriate CoC forms, CoC tape, 

and CoC shipping labels. The cooler lid must be taped completely and the tape signed before 

being shipped. The CoC form used by the USGS National Water Quality Laboratory (NWQL)

can be downloaded at http://wwwnwql.cr.usgs.gov/htmls/cocform.pdf and CoC tape can be 

purchased by USGS employees through the USGS One Stop Store using item number Q150FLD. 

Sediment samples are to be shipped according to U.S. Department of Agriculture (USDA) 

guidelines for shipping regulated soils. Sediment samples must not be shipped in coolers with 

other media (such as water or tissue). The required USDA permit is to be included with all 

sediment samples being shipped to a laboratory.
109 

Table A–1. Sample analyses and laboratories for baseline data collection. 

[USGS, U.S. Geological Survey; PAHs, polycyclic aromatic hydrocarbons; VOCs, volatile organic compounds; TPH GRO + BTEX, total petroleum hydrocarbons –gasoline-range organics plus 

benzene, toluene, ethylbenzene, and zylenes; VOA, volatile organic analysis; NA, not applicable; TN TP TS, total nitrogen, total phosphorus, total sulfur; DOC, dissolved organic carbon; TOC, total 

organic carbon; L, liter; mL, milliliter; oz, ounce]

Laboratory Analysis Matrix Collection method

Laboratory 

schedule/ Code Analytical method

USGS National Water 

Quality Laboratory (NWQL), 

Denver, Colo. 

Semi 

volatiles - 

PAHs Sediment 

1-L glass organic bottle (wide-mouthed), 

100 grams 5506, 5507 

GCMS - 

5506-06 

GS ONWQL

Semi 

volatiles - 

PAHs Whole water 1-L narrow amber glass organic bottle 1383 

GCMS - 

3116-87 

GS ONWQL

Trace 

metals Whole water One 125-mL acid-rinsed bottle 2317 

ICP/MS – GS 

4471-97 

INWQL VOCs Whole water VOC septum vials 2021 

GCMS - 

5506-06 

GS ONWQL Nutrients Whole water

125-mL plastic bottle; H2SO4 (or just chill and 

lab will acidify)

LC2188, 

LC1986, 

LC1984 

EPA 350.1/GS 

Method ID: I4515-91; I-4610-

91 

Test America Labs, Arvada, 

Colo. 

TPH GRO 

+ BTEX Whole water Three VOA vials 50114 8015B 

Test America Labs, Arvada, 

Colo. 

Oil and 

grease Whole water Two 1-L narrow amber glass bottles 50136 1664A 
110 

Table A–1. Sample analyses and laboratories for baseline data collection.—Continued

[USGS, U.S. Geological Survey; PAHs, polycyclic aromatic hydrocarbons; VOCs, volatile organic compounds; TPH GRO + BTEX, total petroleum hydrocarbons –gasoline-range organics plus 

benzene, toluene, ethylbenzene, and zylenes; VOA, volatile organic analysis; NA, not applicable; TN TP TS, total nitrogen, total phosphorus, total sulfur; DOC, dissolved organic carbon; TOC, total 

organic carbon; L, liter; mL, milliliter; oz, ounce]

Laboratory Analysis Matrix Collection method

Laboratory 

schedule/ Code Analytical method

Test America Labs, Arvada, 

Colo.

Oil and 

grease Sediment

One 500-mL amber bed glass organic bottle (widemouthed) (8 oz required, but bottle size not 

available) 50137 9071B

Dr. Arthur

Ga. 

Horowitz, Norcross, 

Trace 

metals, TN, 

TP, TS Sediment

Colorless ziploc bags 

and kept from light – 

– double bagged, chilled, 

500 grams NA (see Appendix C) 

Columbia Environ. Research 

Center, Columbia, Mo. (CERC) Toxicity Sediment 1-L glass bed organic (wide-mouthed) NA (see Appendix C)

Dr. Robert Rosenbauer, 

Menlo Park, Calif.

Oil fingerprinting SedimentTwo 500-mL amber bed glass 

mouthed)

organic bottle (wideNA (see Appendix C)

Dr. Amanda Demopoulus, 

Gainesville, Fla.

Benthic 

invertebrates Sediment 3-inch core 5-cm thick: ziploc bag - chill/freeze NA (see Appendix C)

Dr. John Lisle, 

St. Petersburg, Fla. Bacteria

Land/water 

interface 

(swash) 18-oz WhirlPak or a Ziploc bag - chilled NA

Dry beach sand 18-oz WhirlPak or a Ziploc bag - chilled (see Appendix C)

Dr. George Aiken, Boulder, 

Colo.

DOC - (TOC 

collected)

Whole water

(lab filtered) One 125-mL glass DOC bottle NA (see Appendix C) 

Dr. Robert Eganhouse, 

Reston, Va.

Isomeric 

fingerprinting Whole water 1-L glass bottle NA

Sediment 8-oz wide-mouth jar (see Appendix C)

Dr. Jeff McCoy, NWQL Surfactant Whole water 1-L glass bottle NA (see Appendix C)
111 

Appendix A–2. Pre- and Post-Landfall Sample Analyses and Laboratory Methods

[SVOC, Semi-volatile compounds; PAH, Polyaromatic compounds; NWQL, USGS National Water Quality Laboratory; GCMS, gas 

chromatograph-mass spectrometry; g, gram; L, liter; TAL, TestAmerica Laboratory; oz, ounce; O&G, oil and grease; mL, milliliter; TN, total 

nitrogen; TP, total phosphorus; TS, total sulfur; TOC, total organic carbon; TIC, total inorganic carbon; ; ziplock, Ziplock®; <, less than; μm, 

micrometer; BGC, bottom-material glass container; cm, centimeter; poly, polypropylene plastic container; %, percent; Na, sodium; HCl, 

hydrochloric acid; VOC, volatile organic compounds; BTEX, benzene toluene ethylbenzene and xylenes; VOA, volatile organic analyses; LC, 

laboratory code (NWQL); TPH-GRO, total petroleum hydrocarbons – gasoline range; TPH-DRO, total petroleum hydrocarbons – diesel range; 

ICP/MS, Inductively coupled plasma mass spectrometry; FA, filter-acidify; H2SO4, sulfuric acid; TKN, total kjeldahl nitrogen; NH4, ammonium; 

TOC, total organic carbon; DOC, dissolved organic carbon; DOSS, Di(Ethylhexyl) Sodium Sulfosuccinate.]

Sediment

Sampling

Phase Analysis Laboratory

Method / Laboratory 

Code or Schedule Container Treatment

Pre-landfall SVOC and PAH NWQL GCMS-GS O-5506-06; 

lab codes 5506, 5507

100 g in one 1-L glass, wide 

mouth

Chill.

Post-landfall

Post-landfall

SVOC TAL 8270D One 8-oz glass, wide mouth 

(sample combined in O&G jar)

Chill.

PAH TAL 8270C SIM One 4 oz. glass, wide mouth Chill.

Pre-landfall Oil and Grease TAL 9071B (LC 50137) One 500-mL (8 oz) glass, 

amber, wide mouth

Chill.

Post-landfall Oil and Grease TAL 1664A-HEM One 8 oz. glass, amber, wide 

mouth

Chill.

Pre-landfall Elements and 

TN, TP, TS, 

TOC, TIC

Horowitz (Appendix C) 500 g in colorless ziplock bags, 

doubled.

Chill. Keep away 

from light.

Post-landfall Elements and 

TN, TP, TS, 

TOC, TIC

Horowitz (Appendix C) Two 18 oz. WhirlPak 

sediments

One 18 oz. WhirlPak 

–

– <63 μm

Chill.

Pre-landfall Toxicity Carr and 

Biedenbach

(Appendix C) One 1- L glass (BGC), 

widemouth

Chill.

Post-landfall Toxicity Carr and 

Biedenbach

(Appendix C) Two 1-L glass (BGC), 

widemouth

Chill.

Pre-landfall

Pre-landfall

Bacteria Lisle (Appendix C) One 18 oz. WhirlPak/Ziplock

Swash sediments

Chill.

Bacteria Lisle (Appendix C) One 18 oz. WhirlPak/Ziplock

Dry beach sediments

Chill.

Post-landfall Bacteria Lisle (Appendix C) One 18 oz. WhirlPak 

sediments

– Swash Freeze

Pre-landfall Benthic 

invertebrates

Demopoulos (Appendix C) 3-inch core, 5-cm diameter, in 

ziplock bags.

Chill/Freeze.

Post-landfall Benthic 

invertebrates

Demopoulos (Appendix C) Three 500-mL poly, 

widemouth

Three 500-mL poly, 

widemouth

10% formalin-Na 

borate. Chill.

Chill-unpreserved

Pre-landfall Oil fingerprint Rosenbauer (Appendix C) Two 500-mL glass, amber, 

wide mouth (BGC)

Chill/Freeze.

Post-landfall Oil fingerprint Rosenbauer (Appendix C) Two 500-mL glass, amber, 

widemouth, I-Chem BGC

Freeze.
112 

Appendix A–2. Pre- and Post-Landfall Sample Analyses and Laboratory Methods—

Continued

[SVOC, Semi-volatile compounds; PAH, Polyaromatic compounds; NWQL, USGS National Water Quality Laboratory; GCMS, gas 

chromatograph-mass spectrometry; g, gram; L, liter; TAL, TestAmerica Laboratory; oz, ounce; O&G, oil and grease; mL, milliliter; TN, total 

nitrogen; TP, total phosphorus; TS, total sulfur; TOC, total organic carbon; TIC, total inorganic carbon; ; ziplock, Ziplock®; <, less than; μm, 

micrometer; BGC, bottom-material glass container; cm, centimeter; poly, polypropylene plastic container; %, percent; Na, sodium; HCl, 

hydrochloric acid; VOC, volatile organic compounds; BTEX, benzene toluene ethylbenzene and xylenes; VOA, volatile organic analyses; LC, 

laboratory code (NWQL); TPH-GRO, total petroleum hydrocarbons – gasoline range; TPH-DRO, total petroleum hydrocarbons – diesel range; 

ICP/MS, Inductively coupled plasma mass spectrometry; FA, filter-acidify; H2SO4, sulfuric acid; TKN, total kjeldahl nitrogen; NH4, ammonium; 

TOC, total organic carbon; DOC, dissolved organic carbon; DOSS, Di(Ethylhexyl) Sodium Sulfosuccinate.]

Whole Water

Sampling

Phase Analysis Laboratory

Method / Laboratory 

Code or Schedule Container Treatment

Pre-landfall SVOC NWQL GCMS-GS O-3116-87; 

LC 1383

One 1-L glass, fired, amber jar Chill.

Post-landfall SVOC TAL 8270D Two 1-L glass, fired, amber 

jars

Chill.

Pre-landfall PAH NWQL 1383 One 1-L glass, fired jar Chill.

Pre-landfall Oil and Grease TAL 1664A Two 1-

jars

L glass, fired, amber Chill.

Post-landfall Oil and Grease TAL 1664A One 1-L glass, wide mouth jar Preserved to pH2 

with HCl. Chill.

Pre-landfall VOC (with 

BTEX)

NWQL GCMS – 

LC 2021

GS O-5506-06; Three 40-mL VOA septum 

vials

Chill.

Post-landfall VOC with BTEX TAL 8260B Two 40-mL VOA septum vials Chill.

Pre-landfall TPH-GRO with 

BTEX

TAL 8015B Three 40-mL VOA septum 

vials

Chill.

Post-landfall TPH-GRO TAL 8015B Two 40-mL VOA septum vials Chill.

Post-landfall TPH-DRO TAL 8015B One 1-L glass, fired, amber Chill.

Pre-landfall Trace metals NWQL ICP/MS – 

LC 2317

GS I-4471-97; One 125-mL poly, acid-rinsed 

(FA)

Post-landfall Trace metals TAL 6020 one 250-mL poly, acidified Chill.

Pre-landfall Nutrients NWQL EPA 350.1/GS Method 

ID; I-4515-91; I-4610-91; 

LC 2188, 1986, 1984

One 125-mL poly Add H2SO4 or 

request lab to 

acidify. Chill.

Post-landfall Nutrients (TKN, 

NH4, TP)

TAL 351.2;

365.4

One 250-mL poly, preserved Preserved to 

with H2SO4

pH 2 

Pre-landfall Dissolved organic 

carbon

Aiken (Appendix C) One 125-mL glass, fired, TOC Filter at 

laboratory.

Chill.

Post-landfall Dissolved organic 

carbon

Aiken (Appendix C) One 125-mL glass, fired, DOC Filter in field. 

Chill.

Pre-landfall Surfactant 

(DOSS)

McCoy, NWQL (Appendix C) One 1-L glass, fired Chill/Freeze

Post-landfall Surfactant 

(DOSS)

Furlong, NWQL (Appendix C) Two 1-L Teflon Freeze. Keep from 

light.
113 

Appendix A–3. USGS Gulf of Mexico Pre-Landfall and Post-Landfall Sampling Sites, 2010 Oil Spill. 

Map No.1 Station ID Site Name ("DWH GOM Oil Spill" + name) Lat-dd Long-dd

Sample Date: 

Post-Landfall

Sample Date: 

Pre-Landfall 

FLORIDA

FL-1

FL-2 

FL-3 

FL-4

FL-5

FL-6 

FL-7

FL-8

FL-9 

FL-10

FL-11

FL-12

FL-13

FL-14

FL-15

FL-16

FL-17

FL-18

FL-19

FL-20

FL-21

FL-22

FL-23

FL-24

FL-25

FL-26

302144086581200

302258086263400

301926086091800

300729085440900

294645085243000

294152084460300

300427084105000

290740083031200

285425082412600

273728082441800

263132082114000

255609081440700

251329081101100

243737082522500

254002080092000

260454080063400

264921080021700

244345081000600

265722080045400

265722080045500

243902081332700

243703081323700

243700081322300

273605082454900

300223085260800

244325081351500

Gulf IS NS nr Navarre, FL

Henderson Bch SP nr Destin, FL

Grayton Bch SP nr Seaside, FL

St. Andrews SP nr Panama City,FL

St. Joe P SP nr Port St. Joe, FL

St George IS SP nr E Point, FL

St. Marks NWR nr St. Marks, FL

Piney Pt Bch at Cedar Key, FL

Fort IS Gulf Bch nr Chassah., FL

Fort DeSoto Pk nr St Pete, FL

Captiva IS Bch nr Captiva, FL

Tiger Tail Bch at Marco IS, FL

NW Cape Sable Bch nr Flamingo,FL

Dry Tortugas National Park, FL

B Baggs Cape nr Key Biscayne, FL

Lloyd Bch at Ft Lauderdale, FL

MacArthur Bch at W Palm Bch, FL

Coco Plum Bch nr Marathon, FL

BLM Tract1 nr Jupiter Inlet, FL

BLM Tract2 nr Jupiter Inlet, FL

BLM Tract1 nr Park Key, FL

BLM Tract2 nr Sugarloaf Key, FL

BLM Tract3 nr Sugarloaf Key, FL

BLM Tract at Egmont Key, FL

BLM Lathrop Bayou nr Panama City, FL

Marvin Key at Great White Heron NWR, FL

30.362389

30.382944

30.324056

30.124722

29.779167

29.697861

30.074194

29.127750

28.907194

27.624444

26.525639

25.936139

25.224806

24.627139

25.667417

26.081694

26.822583

24.729250

26.956111

26.956111

24.650556

24.617500

24.616667

27.601389

30.038944

24.709806

-86.970167

-86.442778

-86.155056

-85.736028

-85.408528

-84.767750

-84.180444

-83.053361

-82.690778

-82.738333

-82.194222

-81.734583

-81.169972

-82.873639

-80.155528

-80.109444

-80.038056

-81.169972

-80.081667

-80.081944

-81.557500

-81.543611

-81.539722

-82.763611

-85.435472

-81.644639

10/4/2010

10/5/2010

10/5/2010

10/11/2010

10/13/2010

10/6/2010

10/7/2010

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

not sampled

10/12/2010

not sampled

5/11/10

5/11/10

5/12/10

5/12/10

5/13/10

5/13/10

5/18/10

5/18/10

5/19/10

5/17/10

5/20/10

5/21/10

5/22/10

5/20/10

6/1/10

5/26/10

5/27/10

5/24/10

6/16/10

6/16/10

6/9/10

6/9/10

6/9/10

6/14/10

6/10/10

7/7/10
114 

Appendix A–3. USGS Gulf of Mexico Pre-Landfall and Post-Landfall Sampling Sites, 2010 Oil Spill.—Continued

Map No.1 Station ID Site Name ("DWH GOM Oil Spill" + name) Lat-dd Long-dd

Sample Date: 

Post-Landfall

Sample Date: 

Pre-Landfall 

ALABAMA

AL-1 

AL-2

AL-3 

AL-4 

AL-5

AL-6

AL-7 

AL-8

AL-9

AL-10

301338088193500

301455088110300

301448088044000

301329088003000

301349087541600

301428087434900

301608087345400

301353087561600

301343087520200

301341087495200

West Dauphin Island, AL

Dauphin Is., AL

Dauphin Is., AL

Fort Morgan, AL

Fort Morgan, AL

Gulf Shores AL

Orange Beach AL

BLM-1, AL

BLM-2, AL

Fort Morgan BLM-3, AL

30.227425

30.2488145

30.2468703

30.2249263

30.2304815

30.241314

30.269091

30.2315927

30.2288147

30.228259

-88.326394

-88.184168

-88.077777

-88.00833

-87.904438

-87.730265

-87.581649

-87.937772

-87.867214

-87.831102

10/13/2010

10/7/2010

10/6/2010

10/12/2010

10/13/2010

10/14/2010

10/14/2010

10/13/2010

10/14/2010

10/14/2010

5/8/10

5/9/10

5/9/10

5/8/10

5/8/10

5/8/10

5/8/10

5/24/10

5/24/10

5/24/10

LOUISIANA

LA-22

LA-23

LA-24

LA-25

LA-26

LA-28

LA-29

LA-30

LA-31

LA-32

LA-33

LA-34

LA-35

LA-36

LA-46

LA-6 (Bat06)

294432090083100

294406091511300

292046090254500

293808092460200

291507090551800

293424091321600

294324089432500

294108089234500

291537089570100

291914089105500

293518089364300

300907089144500

285951089085600

285615089235600

294456093394801

292708089521400

Jean Lafitte National Park, LA

Cypremort Point, LA

Lake Felicity, LA

Rockefeller Refuge Beach, LA

Sister Lake, LA

Point Chevreuil, LA

Crooked Bayou, LA

Mississippi R. Gulf Outlet, LA

Grand Isle Bch at State Park, LA

Mississippi R. at Main Pass, LA

Breton Sound, LA

Miss. Sound at Grand Pass, LA

Mississippi R. at South Pass, LA

Mississippi R. at SW Pass, LA

East Sabine, LA

Bay Jimmy at NE Barataria Bay, LA

29.7422222

29.735

29.3461111

29.6355556

29.2519444

29.5733333

29.7233333

29.6855556

29.2602778

29.3205556

29.5883333

30.1519444

28.9975

28.9375

29.7488889

29.4522222

-90.141944

-91.853611

-90.429167

-92.767222

-90.921667

-91.537778

-89.723611

-89.395833

-89.950278

-89.181944

-89.611944

-89.245833

-89.148889

-89.398889

-93.663333

-89.870556

10/13/2010

10/5/2010

10/12/2010

10/7/2010

10/8/2010

10/5/2010

10/13/2010

10/13/2010

10/14/2010

10/7/2010

10/13/2010

10/11/2010

10/7/2010

10/14/2010

10/6/2010

8/23/2010

5/14/10

5/13/10

5/18/10

5/13/10

5/17/10

5/13/10

5/18/10

5/7/10

5/10/10

5/7/10

5/7/10

5/7/10

5/7/10

5/7/10

5/10/10

not sampled
115 

Appendix A–3. USGS Gulf of Mexico Pre-Landfall and Post-Landfall Sampling Sites, 2010 Oil Spill.—Continued

Map No.1 Station ID Site Name ("DWH GOM Oil Spill" + name) Lat-dd Long-dd

Sample Date: 

Post-Landfall

Sample Date: 

Pre-Landfall 

MISSISSIPPI 

MS-37

MS-38

MS-39

MS-40

MS-41

MS-42

MS-43

MS-44

MS-45

301309089044700

301227088582000

301358088533300

301425088440600

301321088353300

301208088253600

301858089141000

302336088535800

302034088325200

South Cat Island Beach, MS

West Ship Island Beach, MS

East Ship Island Beach, MS

West Horn Island Beach, MS

East Horn Island Beach, MS

Petit Bois Island Beach, MS

Pass Christian Beach, MS

BIloxi Beach, MS

Pascagoula Beach, MS

30.2191667

30.2075

30.2327778

30.2402778

30.2225

30.2022222

30.3161111

30.3933333

30.3427778

-89.079722

-88.972222

-88.8925

-88.735

-88.5925

-88.426667

-89.236111

-88.899444

-88.547778

10/14/2010

10/14/2010

10/11/2010

10/12/2010

10/12/2010

10/13/2010

10/8/2010

10/7/2010

10/14/2010

5/7/10

5/7/10

5/7/10

5/8/10

5/8/10

5/8/10

5/8/10

5/8/10

5/8/10

TEXAS 

TX-47 294057093572301 Texas Point, TX

TX-48 295542093521701 Sabine Lake, TX

TX-49 293324094220601 High Island, TX

TX-50 293429094332101 East Bay nr Anahuac, TX

TX-51 291815094461001 Galveston Island, TX

TX-52 294408094501101 Trinity Bay nr Beach City, TX

TX-53 292318094430901 Bolivar Peninsula, TX 

TX-54 292937094544001 Galveston Bay nr Eagle Pt, TX

TX-55 291251094571401 West Bay, Galveston Is SPk, TX

TX-56 290512095063101 San Luis Pass, TX

1 At http://www.usgs.gov/oilspill/ scroll down to “Sampling Efforts.” This will take 

sites, where data for the sites can be accessed. 

29.6825 -93.956389

29.9283333 -93.871389

29.5566667 -94.368333

29.5747222 -94.555833

29.3041667 -94.769444

29.7355556 -94.836389

29.3883333 -94.719167

29.4936111 -94.911111

29.2141667 -94.953889

29.0866667 -95.108611

you to the interactive KMZ link for the 

10/6/2010 5/10/10

not sampled 5/10/10

10/7/2010 5/10/10

not sampled 5/10/10

10/13/2010 5/10/10

not sampled 5/11/10

10/7/2010 5/11/10

not sampled 5/11/10

10/14/2010 5/11/10

10/5/2010 5/11/10

maps identifying these sampling 
116 

Appendix A–4. Maps Showing Locations of USGS Sampling Sites

Figure A–4.1. Locations of the 70 USGS baseline (pre-landfall) sampling sites (shown in red). 

Figure A–4.2. Locations of the USGS post-landfall sampling sites along the 

Florida coastline (shown in white). 
117 

Figure A–4.3. Locations of the USGS post-landfall sampling sites along the 

Alabama and Mississippi coastlines (shown in white). 

 

Figure A–4.4. Locations of the USGS post-landfall sampling sites along the 

Louisiana and Texas coastlines (shown in white). 
118 

Appendix B. Field Supplies Recommended for the October 2010 OilSpill Sampling.

[GOM, Gulf of Mexico; #, number; e.g., for example; DEET, N,N-Diethyl-meta-toluamide;HCl, hydrochloric acid; ASR/CoC, Analytical 

Services Request/Chain of Custody; EZ, exclusion zone; CRZ, contaminant reduction zone; poly, polyethylene; DOT, U.S. Department of 

Transportation; DO, dissolved oxygen; SC, specific electrical conductance; NFM, USGS National Field Manual for the Collection of WaterQuality Data; NWQL, USGS National Water Quality Laboratory; TAL, TestAmerica Laboratory; WSC, USGS Water Science Center; OWQ, 

USGS Office of Water Quality; mil, 1/1000th of an inch in thickness; in, inch] 

General Field Equipment/Supplies Description Description/Source/Comment

Personal Protective Equipment (PPE)

Photoionization Detector (PID) 

with calibration gases

With or without 

explosimeter Rent or purchase

Safety glasses/goggles

Laboratory/field 

safety GSA/open market

Elbow/shoulder 

coated gloves

length rubberPPE – field safety http://www.labsafety.com/search/rubber+

shoulder/24543486/2056/?GoButton=

Go&isredirect=true

Disposable nitrile gloves

Laboratory/field 

safety

USGS One-Stop Shop (access restricted to 

USGS)

Tyvek pants and(or) coveralls PPE – field safety

http://www.labsafety.com/search/tyvek+

pants/24532559/

Latex overboots (waterproof) PPE – field safety Open market

Duct or Chemron tape PPE – field safety Open market

PFD (cleanable) – Type 5- 

Revere Model 280 Work Vest

Nylon buckle 

closure, modified as 

described in Section 

3.4

Model #10967776; 

http://www.portsupply.com/webapp/wcs/stores/

servlet/TopCategoriesDisplay?langId=-

1&storeId=50005&catalogId=10001

PFD - Type 3 PPE – field safety USGS standard issue

Waders/ hip boots (rubberized) PPE – field safety Open market

Sterile latex surgical gloves PPE – field safety Fisher Scientific, catalog # 19-014-641

Insect repellent (noncontaminating) PPE – field safety Without DEET

Steel-toes shoes/boots & hard hat PPE – field safety As specifically required by the work task.

Cleaning/Decontamination Supplies

Marble chips or baking soda Neutralization of acid solutions

Nonphosphate detergent and 

degreaser 

Examples: LiquiNox, Dawn, Simple 

Green Open market

Spray bottles Open market

Buckets, three to five 

5-gallon, with lids 

and handles Open market

Long handled brushes Open market

Short handled brushes Open market

Bottle brushes Open market

Soft paint brush Open market

Cotton swabs, pipe cleaners Open market

Plastic sheeting Cover CRZ Open market

Kimwipes, WypAll X70 cloths

Water sampling and 

cleaning Open market

Roll of police-barrier tape

To delineate EZ, 

CRZ Open market
119 

Appendix B. Field Supplies Recommended for the October 2010 OilSpill Sampling.—Continued

[GOM, Gulf of Mexico; #, number; e.g., for example; DEET, N,N-Diethyl-meta-toluamide;HCl, hydrochloric acid; ASR/CoC, Analytical 

Services Request/Chain of Custody; EZ, exclusion zone; CRZ, contaminant reduction zone; poly, polyethylene; DOT, U.S. Department of 

Transportation; DO, dissolved oxygen; SC, specific electrical conductance; NFM, USGS National Field Manual for the Collection of WaterQuality Data; NWQL, USGS National Water Quality Laboratory; TAL, TestAmerica Laboratory; WSC, USGS Water Science Center; OWQ, 

USGS Office of Water Quality; mil, 1/1000th of an inch in thickness; in, inch] 

General Field Equipment/Supplies Description Description/Source/Comment

Cleaning/Decontamination Supplies—continued

Pressure sprayers Open market

DOT-certified metal/plastic 

containers Liquid waste Open market

Spray/squeeze bottles/dispensers

Poly and Teflon to 

contain deionized 

and blank water Open market

Trash bags and containers

Solid waste; cover 

cleaned equipment Open market

Methanol, laboratory-grade Pesticide grade Open market

HCl, 5-percent solution High-purity grade Open market

Tap water Potable quality Open market

Heating plate, stir bars Portable Open market

Sample-Collection, Processing, Preservations

Multiparameter instrument and 

sensors: Turbidity, DO, pH, 

Temperature, SC See NFM Chapter 6

Open market; DO luminescent technology 

sensor 

Calibrants for sonde sensors Open market

YSI C-spray coating Sonde protection

YSI, 

https://www.ysi.com/accessoriesdetail.php?Ant

i-fouling-C-Spray-Protective-Probe-Solution129

Plastic bags, ziplock bags

Ice, sample 

containers Open market

Rubber bands Heavy duty Open market

Aluminum foil

Cover Teflon sample 

bottles Open market

Field Form

Customized for 

project

OWQ_Deep_Oil 

restricted) 

website (my.usgs.gov–access 

GPS

Field Logbook and indelible pen

Bound, paginated, 

“rite in the rain,”

Poly cover

http://www.riteintherain.com/

ItemForm.aspx?item=550&Category=

6fd10376-a439-4797-95f0-349a58e602ea

ASR/CoC Forms

Customized for 

project

OWQ_Deep_Oil 

access) 

wiki (my.usgs.gov – restricted 

Replacement brushes and wipers

For multiparameter 

sonde Open market

Tape measure (0.01-ft graduations) Open market

Metal or wooden stakes

PVC tube sampling 

method Open market

Digital camera Site & sample photos Open market

Sledge hammer, spade/shovel Site preparation Open market
120 

Appendix B. Field Supplies Recommended for the October 2010 OilSpill Sampling.—Continued

[GOM, Gulf of Mexico; #, number; e.g., for example; DEET, N,N-Diethyl-meta-toluamide;HCl, hydrochloric acid; ASR/CoC, Analytical 

Services Request/Chain of Custody; EZ, exclusion zone; CRZ, contaminant reduction zone; poly, polyethylene; DOT, U.S. Department of 

Transportation; DO, dissolved oxygen; SC, specific electrical conductance; NFM, USGS National Field Manual for the Collection of WaterQuality Data; NWQL, USGS National Water Quality Laboratory; TAL, TestAmerica Laboratory; WSC, USGS Water Science Center; OWQ,

USGS Office of Water Quality; mil, 1/1000th of an inch in thickness; in, inch] 

General Field Equipment/Supplies Description Description/Source/Comment

Sample-Collection, Processing, Preservations—continued

Bucket, 2.5-gallon, for sediment 

Process sediment 

sample Open market

Teflon bucket liners 

Sediment collection 

bucket

OWQ to provide directly from 

one use per site (disposable)

manufacturer; 

Teflon bags (small) Open market; one use per site (disposable)

Polycarbonate core tubes Invertebrate samples OWQ to provide directly from manufacturer

Teflon sampling scoop

Make from Teflon 

bottles; collect, 

homogenize 

sediments

NWQL--Constructed by WSC from Teflon 

bottle; clean between sites or one use per site 

(disposable)

Teflon coring tubes and plates

Collect and contain 

sediments 

OWQ to provide directly from manufacturer; 

one use per site (disposable) or clean between 

sites if reused.

Peristaltic pump & pump carrier Open market

C-flex tubing, cleaned 

Cut to ~ 8-ft lengths 

or greater, as needed

Length required can depend on deployment 

method; one use per site (disposable)

WhirlPaks, 18 ounce

Bacteria, sediment 

metals and nutrients NFSS oil-spill kit (Q613fld) or open market

Sample bottles/containers 

See Appendix D for 

container 

requirements

Oil-spill kit from One-stop Q613FLD; TAL 

supplies bottles & preservatives for their 

analyses

Preservation chamber and

bag

chamber To collect equipment 

blank 

See NFM chapters 3, 4, 5; 

(disposable)

one use per site 

Hydrochloric acid, sulfuric acid, and 

nitric acid sample preservative

Chemical 

preservatives

Backup / extra ampoules from NWQL; not 

needed if sample bottles from TAL contain 

preservative

10-percent formalin, saturated 

sodium borate 

with Preserve invertebrate 

samples Open market

Holder/flotation device for samples Water sampling Open market

Winkler kit and calibration solutions Check sonde DO Open market

PVC tube, 4 in. diam., ~2-3 ft. long; 

and stainless steel O clamps 

PVC-tube sampling 

method Open market

pH test strips 

Check oil and

sample pH

grease 

Open market; not for official pH report

Tape: duct, electrical, Teflon

Seal lids to 

containers Open market

Coolers Non-leaking Open market

Shipping

Labels (sample container, shipping) Open market

FedEx Airbills Federal Express (FedEx)

Coolers Open market

Wet ice (label field form “ice”) Open market
121 

Appendix B. Field Supplies Recommended for the October 2010 OilSpill Sampling.—Continued

[GOM, Gulf of Mexico; #, number; e.g., for example; DEET, N,N-Diethyl-meta-toluamide;HCl, hydrochloric acid; ASR/CoC, Analytical 

Services Request/Chain of Custody; EZ, exclusion zone; CRZ, contaminant reduction zone; poly, polyethylene; DOT, U.S. Department of 

Transportation; DO, dissolved oxygen; SC, specific electrical conductance; NFM, USGS National Field Manual for the Collection of WaterQuality Data; NWQL, USGS National Water Quality Laboratory; TAL, TestAmerica Laboratory; WSC, USGS Water Science Center; OWQ,

USGS Office of Water Quality; mil, 1/1000th of an inch in thickness; in, inch] 

General Field Equipment/Supplies Description Description/Source/Comment

Shipping—continued

Dry Ice (label field form “dry ice”) Open market

Liners for

ice

cooler, plastic bags for 

Open market

Foam/bubble sleeves 

Bubble Bag 

6-in by 8-in

NFSS oil-spill kit (Q613fld) or open market; 

http://www.uline.com/, catalog #S-5990

Dry-Ice stickers Place on cooler Open market

Nylon reinforced tape Wrap around cooler Open market

CoC tape Wrap around cooler

USGS One-Stop Shop (#Q150FLD) or open 

market

CoC label Open market, or prepared by WSC

Paper towels Open market

Ziplock plastic bags-4-mil strength Open market
122 

Appendix C. Research Methods

Appendix Research Method Chief 

Scientist(s)

C-1. DOC Analysis of Gulf of Mexico nearshore water 

samples for dissolved organic carbon quantity 

and quality utilizing absorbance and 

fluorescence spectroscopy

G.R. Aiken 

C-2. Toxicity Sediment toxicity tests of beach and wetland 

samples collected in response to the 

Deepwater Horizon oil release, Gulf of 

Mexico, 2010

R.S. Carr and J.M. 

Biedenbach 

C-3. Benthic 

Invertebrates

Investigation of benthic invertebrates in beach 

and wetland samples collected pre- and postlandfall of the Deepwater Horizon oil release 

to the Gulf of Mexico, 2010 

A.W.J. 

Demopoulos 

C-4. DOSS Forensic research for determination of 

Di(ethylhexyl) Sodium Sufosuccinate (DOSS),

an anionic surfactant in Corexit® released to 

the Gulf of Mexico, 2010

J.L. Gray and 

E.T. Furlong

C-5. Trace and 

Major Elements 

and Nutrients

Analysis of Gulf of Mexico coastal sediments 

for trace elements, major elements, and 

nutrients, pre- and post-landfall of the 

Deepwater Horizon oil spill, 2010

A.J. Horowitz

C-6. Bacteria Microorganisms in pre- and post-oiled coastal 

sediments, Gulf of Mexico, 2010

J.T. Lisle

C-7. Oil 

Fingerprint

Fingerprint analysis of oil in sediment and 

tarballs from the northern Gulf of Mexico 

shoreline, 2010

R.J. Rosenbauer
123 

Appendix C-1. Analysis of Gulf of Mexico Nearshore Water Samples for Dissolved 

Organic Carbon Quantity and Quality Utilizing Absorbance, Fluorescence, and Low 

Pressure Chromatography with XAD Resins

Chief Scientist: G.R. Aiken – USGS, Boulder, Colo.

Method Description: 

Dissolved organic matter (DOM) plays an important role in coastal ecosystems as a source of 

carbon for microorganisms. As hydrocarbon-rich oil infiltrates the Gulf of Mexico, studying the 

quantity and quality of DOM will provide insight as to the ecological effects of the spill. The fate 

and transport of the oil, as well conversion of the oil to DOM by microorganisms can be 

measured utilizing a variety of quantitative and qualitative techniques. Absorbance is a 

qualitative measure of dissolved organic carbon (DOC), and the ratio of absorbance at the 

wavelength 254 nm to the concentration of DOC in the water, known as the Specific Ultraviolet

Absorbance (SUVA254nm), has been highly correlated to percent aromaticity by 13C NMR. Oil 

and oil additives contain highly fluorescent compounds that have a prolonged breakdown 

process. Thus, fluorescence is being used to track oil-related fluorophores by measuring 

Excitation-Emission Matrices (EEMs) of water samples. 

For samples with chloride concentrations < 0.02M, DOC concentration will be analyzed using 

the heated persulfate oxidation method of the OI Analytical Model 700 instrument. All other 

samples will be analyzed on a Shimadzu TOC-V carbon analyzer which uses the combustion 

method of oxidation. (Aiken, 1992), Data are reported to +- 0.2 mg/L C. Absorbance scans 

(wavelengths 200 to 800 nm, every 1 nm) will be measured on an HP8453 UV-Vis 

Spectrophotometer, which utilizes a photodiode array. Absorbance data produced are unitless

and are reported to +- 0.002. SUVA254nm will then be calculated for each sample (Weishaar and 

others, 2003). Fluorescence EEMs will be measured on a JY Horiba Fluoromax-3 or Fluoromax4. Samples will be excited every 5 nm from 240 to 450 nm, and emission scans will be collected 

every 2 nm from 300 to 600 nm (Murphy and others, 2010). 

• Aiken, G.R., 1992, Chloride interference in the analysis of dissolved organic carbon by 

the wet oxidation method: Environmental Science and Technology, v. 26, p. 2435-2439. 

• Murphy, K.R., Butler, K.D., Spencer, R.G.M., Stedmon, C.A., Boehme, J.R., Aiken, G.R., 

The measurement of dissolved organic matter fluorescence in aquatic environments: An 

interlaboratory comparison. Environ. Sci. Technol. 2010, 44, 9405–9412. 

• Weishaar, J.L., Aiken, G.R., Bergamaschi, B.A., Fram, M.S., Fujii, R., and Mopper, K., 

2003, Evaluation of specific ultraviolet absorbance as an indicator of the chemical 

composition and reactivity of dissolved organic carbon: Environmental Science and 

Technology, v. 37, no. 20, pp. 4702-4708. 
124 

Appendix C-2. Sediment Toxicity Tests of Beach and Wetland Samples Collected in 

Response to the Deepwater Horizon Oil Release, Gulf of Mexico, 2010

Chief Scientists: R.S. Carr and J.M. Biedenbach – USGS Columbia Environmental Research Center, 

Marine Ecotoxicology Research Station, Corpus Christi, Tex. 

Method Description: 

Fertilization and embryological development tests with the sea urchin, Arbacia punctulata. 

These tests will compare the toxicity of the test samples with a reference sample. We have 

specific standard operating procedures for all our methods (unpublished). The precision of these 

tests has been described in Carr and Biedenbach 1999. A phase one toxicity identification 

evaluation (TIE) will be performed using the fertilization or embryological development tests on 

any available toxic post-impact samples to determine the class or classes of chemicals 

contributing to the observed toxicity (EPA, 1996). 

• Carr, R.S. and J.M. Biedenbach. 1999. Use of power analysis to develop detectable 

significance criteria for sea urchin porewater toxicity tests. Aquat. Ecosyst. Hlth. Mngmt. 

2:413-418. 

• EPA. 1996. Marine Toxicity Identification Evaluation (TIE): Phase I Guidance Document. 

EPA/600/R-96/054. Office of Research and Development, Washington, D.C. 

• A citation for the porewater method in general is : 

− Carr, R.S. 1998. Sediment porewater testing. In: Standard Methods for the 

Examination of Water and Wastewater, section 8080, 20th Edition, Clesceri, L.S., 

A.E. Greenberg, and A.D. Eaton (eds.), American Public Health Association, 

Washington, DC., pg. 8-37 to 8-41. 

• A citation for abbreviated description of the sea urchin porewater tests is: 

Carr, R.S., P.A. Montagna, J.M. Biedenbach, R. Kalke, M.C. Kennicutt, R. Hooten, and 

G. Cripe. 2000. Impact of storm water outfalls on sediment quality in Corpus Christi 

Bay, Texas. Environ. Toxicol. Chem. 19:561-574. 
125 

Appendix C-3. Investigation of Benthic Invertebrates in Beach and Wetland Samples 

Collected Pre- and Post-Landfall of the Deepwater Horizon Oil Release to the Gulf of 

Mexico, 2010 

Chief Scientist: A.W.J. Demopoulos – USGS, Gainesville, Fla.

Method Description: 

See: Demopoulos, A.W.J., and Smith, C.R., 2010, Invasive mangroves alter macrofaunal 

community structure and facilitate opportunistic exotics in Marine Ecology-Progress Series 404: 

51-67 2010. 

Appendix C-4. Forensic Research for Determination of Di(Ethylhexyl) Sodium 

Sulfosuccinate (DOSS), an Anionic Surfactant in Corexit Dispersants Released to the 

Gulf of Mexico, 2010

Chief Scientists: J.L. Gray and E.T. Furlong – USGS National Water Quality Laboratory, Denver, Colo.

Method Description:

The purpose of this forensic research is development of an analytical method to analyze for 

residual concentrations of di(ethylhexyl) sodium sulfosuccinate (DOSS), a primary surfactant 

component in the Corexit® dispersants used by BP in addressing the Deepwater Horizon oil spill 

to the Gulf of Mexico in 2010. Standards for surfactant compounds formulated into Corexit®

9500 and 9527, as well as reference samples of Corexit® dispersants, are being used to determine 

retention-time data and reference mass spectra for the DOSS in the Corexit® dispersants. 

The following publications illustrate the forensic approach for liquid chromatography: 

• Ferrer, I, Schroder, H., and Furlong, E., "Atmospheric Pressure Ionization Mass 

Spectrometry - IX. LC-MS Analysis of Cationic Surfactants: Methods and Applications", 

in "Analysis and Fate of Surfactants in the Aquatic Environment", Knepper, T., Barcelo, 

D. and De Voogt, P., Elsevier, p. 353-383, 2003. 

• Furlong, E., Ferrer, I., Gates, P., Cahill, J. and Thurman, M., "Identification of Labile 

Polar Organic Contaminants by Atmospheric-Pressure Tandem Mass Spectrometry", in 

Liquid Chromatography/Mass Spectrometry, MS/MS and Time of Flight MS", Ferrer, I. 

and Thurman, M., eds., ACS Symposium Series 850, p. 175-187, 2003.
126 

Appendix C-5. Analysis of Gulf of Mexico Coastal Sediments for Trace Elements, 

Major Elements, and Nutrients, Pre- and Post-Landfall of the Deepwater Horizon Oil 

Spill, 2010

Chief Scientist: A.J. Horowitz – USGS, Norcross, Ga.

Method Description:

Bulk and a less-than 63-micrometer aliquot of bed-sediment samples are dried and analyzed for a 

large group of elements (listed below). The data that result are used to establish pre-oiling 

baseline values for the various site locations and compared with data resulting from analysis of 

sediments from the same locations after landfall of the oil. The data sets are analyzed to 

determine if there are any statistically significant chemical differences between the two data sets. 

The same analytical procedures have been used in previous studies that were subject to legal 

scrutiny and action. 

Trace and major elements: Ag, Cu, Pb, Zn, Cd, Cr, Co, Ni, Ba, V, Li, Be, Mo, Sr, As, Sb, Se, 

Hg, Fe, Mn, Al, and Ti. 

Nutrients: TN, TP, TS, TC, TOC, and TIC.

• For all chemical elements other than As, Sb, Se, and Hg, 500-mg aliquots, are digested 

with a combination of HF/HClO4/aqua regia in Teflon® beakers at 200°C; the resulting 

salts are solubilized using 50 mL of 2 percent HCl.

• Ag, Cd, and Pb are determined by flame atomic absorption spectrometry (AAS) using 

mixed salt standards and background correction. 

• All the other constituents are determined by inductively coupled plasma-atomic emission 

spectroscopy (ICP-AES) using a lutetium internal standard and interelement correction 

factors. 

− Aliquots from the same digestion are used for As, Sb, and Se by hydride generation 

ICP-AES. 

− Hg is analyzed using separate 500-mg aliquots digested with LeFort aqua regia at 

140°C; quantification is by cold vapor, employing an AAS as the detector. 

− TC and TN are determined by passing the combustion products of separate 250- to 

500-mg sample aliquots through a gas chromatograph, with a thermal conductivity 

detector in a C/N/S analyzer. 

− TOC also is determined by combustion, but in a C/S analyzer that quantifies the 

evolved CO2 with an infrared detector after pretreatment with 10 percent volume-tovolume HCl to remove inorganic carbonates. 
127 

• Horowitz, A.J., Elrick, K.A., and Smith, J.J., 2001, Hydrological Processes, 15, 1107- 

1132. 

• Fishman, M.J. and Friedman, L.C., 1989, Methods for Determination of Inorganic 

Substances in Water and Fluvial Sediments, USGS TWRI Book 5, 545 p. 
128 

Appendix C-6. Microorganisms in Pre- and Post-Oiled Coastal Sediments of the Gulf 

of Mexico, 2010

Chief Scientist: J.T. Lisle – USGS, St. Petersburg, Fla.

Method Description:

Phase 1 of this work focuses on using polymerase chain reaction (PCR) and denaturing gradient 

gel electrophoresis (DGGE) to provide a genetic “fingerprint” of the microbial communities that 

naturally inhabit the coastal sediments that have not been contaminated with oil from the 

Deepwater Horizon/BP event. Nucleic acid sequencing methods are being used to identify some 

of the microbial species within these communities that may or may not be capable of degrading 

crude oil. These microbial community fingerprints will be compared to chemical fingerprints of 

oil or oil-degradation products in the same samples (see oil-fingerprint research by Dr. Robert 

Rosenbauer, USGS, Menlo Park). Collectively, the data from these analyses will provide a 

microbial and geochemical baseline by which to compare the post-oiled sediment samples. 

Phase 2 of this study focuses on monitoring the progress and efficiency of remediation processes 

along coastal zones that have been contaminated with oil. The same microbiology and 

geochemical methods will be used as are described for Phase 1, but the samples will be analyzed 

over an extended period of time. Because of the natural succession of microbial communities 

that preferentially degrade constituents of crude oil into smaller and less toxic by-products, the 

goals for this phase of the study are (1) to determine the overall rates and efficiencies of 

bioremediation processes, (2) identify the microbial genera/species responsible for the respective 

steps in the overall degradation process, and (3) determine the oil constituents and/or degradation 

by-products that are being preferentially degraded further or that become recalcitrant to 

bioremediation. This approach will allow the USGS to objectively monitor the oil spill cleanup 

efforts along impacted coastal zones. All appropriate controls will be run to assure the reliability 

of the resulting data.

References that describe the microbiology and geochemical methods:

• MacNaughton, S.J., and others, (1999). Microbial population changes during bioremediation 

of an experimental oil spill. Applied and Environmental Microbiology. 65(8):3566-3574. 

• Roling, W., and others, (2004). Bacterial community dynamics and hydrocarbon degradation 

during a field-scale evaluation of bioremediation on a mudflat beach contaminated with buried 

oil. Applied and Environmental Microbiology. 70(5):2603-2613. 

• Alonso-Gutierrez, J., and others, (2008). Alcanivorax strain deteted among the cultured 

bacterial community from sediments affected by the Prestige oil spill. Marine Ecology 

Progress Series. 362:25-36.

• Gertler, C., and others, (2009). Microbial consortia in mesocosm bioremediation trial using oil 

sorbents, slow-release fertilizer and bioaugmentation. FEMS Microbiology Ecology. 69:288-

300. 
129 

Appendix C-7. Fingerprint Analysis of Oil in Sediment and Tarballs from the 

Northern Gulf of Mexico Shoreline, 2010

Chief Scientist: R. J. Rosenbauer – USGS, Menlo Park, Calif.

Method Description:

The organic chemical and isotopic composition of the sediment, including biomarkers of any 

petroliferous component, will be determined. In brief, organic chemical analyses are carried out 

by gas chromatography/mass spectroscopy following accelerated microwave-assisted solvent 

extraction and compound fractionation by liquid column chromatography. Biomarker values are 

used to correlate the samples and group them according to their probable sources (Peters and 

others, 2008; Lorenson and others, 2009). 

• Rosenbauer, R.J. and others, 2011, Petroleum Hydrocarbons in Sediment from the 

Northern Gulf of Mexico Shoreline, Texas to Florida, U.S. Geological Survey Open-File 

Report 2011-1014, 22 p., accessed online at 

http://pubs.er.usgs.gov/publication/ofr20101290/.

• Rosenbauer, R.J. and others, 2010, Reconnaissance of Macondo-1 well oil in sediment and 

tarballs from the northern Gulf of Mexico shoreline, Texas to Florida: U.S. Geological Survey 

Open-File Report 2010-1290, 22 p., accessed online at http://pubs.usgs.gov/of/2010/1290/. 

• Lorenson, T.D. and others, 2009, Natural offshore oil seepage and related tarball accumulation 

on the California coastline—Santa Barbara Channel and the Southern Santa Maria Basin; 

source identification and inventory: U.S. Geological Survey Open-File Report 2009-1225, 116 

p.

• Kvenvolden, K.A. and others, 2002. Hydrocarbons in recent sediment of the Monterey 

Bay National Marine Sanctuary, Marine Geology 181, 101-113. 
130 

Appendix D. Post-Landfall Shipping Requirements for Water and 

Sediment Samples 

Table D–1. Post-landfall water samples: Laboratory, sample, shipping, and 

quality-control requirements.

Table D–2. Post-landfall sediment samples: Laboratory, sample, shipping, and 

quality-control requirements.

Tables D–1 and D–2 that follow are provided as examples only and contain information 

specific to USGS Deepwater Horizon, Gulf of Mexico, 2010, post-landfall sample collection.
131 

Table D–1. Post-landfall water samples: Laboratory, sample, shipping, and quality-control requirements.

SHIPPING: FEDEX 

PRIORITY OVERNIGHT Quality Control Samples* PROTECT SAMPLES SHIPPING ADDRESS and CONTACT 

FROM CONTACT WITH INFORMATION 

COLLECTION and ICE MELTWATER: 

CONTAINER VOLUME PRESERVATION Double-bag and seal NOTE SHIPPING INSTRUCTIONS AND 

AND TYPE -- Wipe all containers each sample using CONTACTS FOR SATURDAY DELIVERIES. LABORATORY ANALYSIS clean and dry, check heavy-duty ziplock bags When shipping on a Friday,

label before packing. and double-bag the ice on airbill under “Special Handling,” 

(total of 4-bag layer mark "Saturday delivery." (Do NOT 

between ice and mark "hold for Saturday")

containers). ENSURE 

THAT COOLERS ARE 

LEAK-PROOF. 

303-236-3181; FAX 303.236.3719 Leave sufficient Keep sample bottles paalex@usgs.gov headspace for freezing UPRIGHT. FREEZE LOGIN, National Water Quality √ √ sample. Wipe bottles or ship same day on ice. Dr. Ed Furlong, Two 1-L Teflon Laboratory, USGS, Att: Furlong, Federal free of oil and water. Include return address NWQL, Denver, bottles (from NWQL) Center, Bldg 95, MS 407—Entrance E3, Wrap in clean label and account Colo. – Surfactant Denver Federal Center, Denver CO, aluminum foil. KEEP number. Include 80225-0046. (For Saturday delivery, BOTTLE Return-FedEx airbill NWQL arranges sample pickup at UPRIGHT. with CoC paperwork. Fedex)

Collect raw sample in 303-541-3009, graiken@usgs.gov 500-mL baked amber CHILL to 4°C. Place USGS, Attn: Kenna Butler, Suite E127, glass. Rinse the filter sample bottle in foam √ √ 3215 Marine St, Boulder, CO 80303. 125-mL DOC bottle. with 50 mL of IPBW or bubble sleeve and Address for Saturday delivery: LOGIN, Use 500 mL glass to and 50 mL sample; fill seal in ziplock bags. Dr. George Aiken, National Water Quality Laboratory, collect. Analysis: 125-mL DOC bottle, DO NOT FREEZE. Boulder, Colo. USGS, Att: Aiken/Butler, Bldg 95, MS Dissolved Organic leaving headspace. Ship chilled at 4°C. 407--Entrance E3, Denver Federal Carbon Chill and maintain at Include Return-FedEx Center, Denver CO, 80225-0046. Will be or less than 4°C airbill with CoC picked up at Fedex. Contact: Pat Alex, without freezing. Ship paperwork. 303-236-3181, paalex@usgs.gov overnight. Equipment Blank Water Equipment Blank Sediment Duplicate Ambient Blank

Matrix Spike (not oiled site)

 
132 

Table D-1. Post-landfall water samples: Laboratory, sample, shipping, and quality-control requirements —Continued.

SHIPPING: FEDEX 

PRIORITY OVERNIGHT Quality Control Samples* PROTECT SAMPLES SHIPPING ADDRESS and CONTACT 

FROM CONTACT WITH INFORMATION 

COLLECTION and ICE MELTWATER: 

CONTAINER VOLUME PRESERVATION Double-bag and seal NOTE SHIPPING INSTRUCTIONS AND 

AND TYPE -- Wipe all containers each sample using CONTACTS FOR SATURDAY DELIVERIES. LABORATORY ANALYSIS clean and dry, check heavy-duty ziplock bags When shipping on a Friday,

label before packing. and double-bag the ice on airbill under “Special Handling,” 

(total of 4-bag layer mark "Saturday delivery." (Do NOT 

between ice and mark "hold for Saturday")

containers). ENSURE 

THAT COOLERS ARE 

LEAK-PROOF. 

CHILL to 4°C. Place See Protocol Section 6 sample bottle in foam or for collection Two 40-mL VOA bubble sleeve and in √ √ √ √ methods. Ensure vials w/septum. sealed ziplock bags. absence of bubbles in Analysis: TCL VOCs Ship priority sample. Unpreserved. (Method 8260B) overnight, protected TAL (Test Chill to 4°C without from meltwater and in a America freezing. leakproof cooler. Laboratories), CHILL to 4°C. Place Pensacola, Fla. 850-471-6227 sample bottle in foam or ALL See Protocol Section 6 Two 40-mL VOA bubble sleeve and in √ √ √ √ CONTAINERS for collection marty.edwards@testamericainc.com vials w/septum. sealed ziplock bags. (EXCEPT "RA") methods. Ensure Analysis: TPH GRO Ship with VOCs, ARE SUPPLIED absence of bubbles in Marty Edwards (C6-C10) (Method priority overnight, BY TAL, PLUS sample. Unpreserved. 3355 Mclemore Drive 8015B) protected from ONE VOC TRIP Chill to 4°C. Pensacola, FL 32514 meltwater and in a BLANK AND ONE leakproof cooler. TEMPERATURE One 1-L fired amber CHILL to 4°C. BLANK glass. Bubble wrap, place in Unpreserved. Fill, Analysis: TPH Diesel ziplock bags and seal. √ √ √ √ √ leaving headspace. and Oil-range organics Ship priority overnight, Chill to 4°C without (DRO/ORO) w/ protected from freezing. chromatograms meltwater and in a 

(Method 8015B). leakproof cooler.

Equipment Blank Water

Equipment Blank Sediment

Duplicate

Ambient Blank

Matrix Spike (not oiled site)

 

 

 
133 

Table D-1. Post-landfall water samples: Laboratory, sample, shipping, and quality-control requirements —Continued.

LABORATORY

CONTAINER VOLUME 

AND TYPE -- 

ANALYSIS

COLLECTION and 

PRESERVATION 

Wipe all containers 

clean and dry, check 

label before packing.

SHIPPING: FEDEX 

PRIORITY OVERNIGHT 

PROTECT SAMPLES 

FROM CONTACT WITH 

ICE MELTWATER: 

Double-bag and seal 

each sample using 

heavy-duty ziplock bags 

and double-bag the ice 

(total of 4-bag layer 

between ice and 

containers). ENSURE 

THAT COOLERS ARE 

LEAK-PROOF.

SHIPPING ADDRESS and CONTACT 

INFORMATION 

NOTE SHIPPING INSTRUCTIONS AND 

CONTACTS FOR SATURDAY DELIVERIES. 

When shipping on a Friday,

on airbill under “Special Handling,” 

mark "Saturday delivery." (Do NOT 

mark "hold for Saturday")

Quality Control Samples* Equipment Blank Water Equipment Blank Sediment Duplicate Ambient Blank Matrix Spike (not oiled site)

TAL (Test 

America 

Laboratories), 

Pensacola, Fla. 

ALL 

CONTAINERS 

(EXCEPT "RA") 

ARE SUPPLIED 

BY TAL, PLUS 

ONE VOC TRIP 

BLANK AND ONE 

TEMPERATURE 

BLANK

Two -L fired amber 

glass. 

Analysis: 

Semivolatile Organic 

Compounds (SVOC 

TCL) (Method 

8270D)

Unpreserved. Fill, 

leaving headspace. 

Chill to 4oC without 

freezing. 

CHILL to 4oC. 

Bubble wrap, place in 

sealed ziplock bags. 

Ship priority overnight, 

protected from 

meltwater and in a 

leakproof cooler.

850-471-6227

marty.edwards@testamericainc.com

Marty Edwards 

3355 Mclemore Drive 

Pensacola, FL 32514

√ √ √ √ √

One 1-L (32 oz) clear 

wide mouth glass. 

Analysis: Oil and 

Grease HEM 

(Method 1664A)

Preserved with HCl. 

Fill, leaving headspace. 

If HCl is lost, check 

that pH < 2, and add if 

needed. Chill to 4oC 

without freezing.

CHILL to 4oC. Bubble 

wrap, place in ziplock

bags and seal. Ship 

priority overnight, 

protected from 

meltwater and in a 

leakproof cooler.

√ √ √ √

250-mL poly, prepreserved with HNO3

for Metals/Trace 

Elements analysis. 

One 1-L RA ("raw, 

acidified") poly bottle 

from NWQL for 

sample collection. 

Use precleaned, 

blanked 

1-L RA bottle to collect 

dip sample and fill acidpreserved 250-mL poly 

bottle. Leave 

headspace. Check pH 

and add HNO3 to pH < 

2, if needed. Chill to 

4oC without freezing.

CHILL to 4oC. Place 

in sealed plastic bag. 

Ship priority overnight, 

protected from 

meltwater and in a

leakproof cooler.

√ √ √ √
134 

Table D-1. Post-landfall water samples: Laboratory, sample, shipping, and quality-control requirements —Continued.

LABORATORY

CONTAINER VOLUME 

AND TYPE -- 

ANALYSIS

COLLECTION and 

PRESERVATION 

Wipe all containers 

clean and dry, check 

label before packing.

SHIPPING: FEDEX 

PRIORITY OVERNIGHT 

PROTECT SAMPLES 

FROM CONTACT WITH 

ICE MELTWATER: 

Double-bag and seal 

each sample using 

heavy-duty ziplock bags 

and double-bag the ice 

(total of 4-bag layer 

between ice and 

containers). ENSURE 

THAT COOLERS ARE 

LEAK-PROOF. 

SHIPPING ADDRESS and CONTACT 

INFORMATION 

NOTE SHIPPING INSTRUCTIONS AND 

CONTACTS FOR SATURDAY DELIVERIES. 

When shipping on a Friday,

on airbill under “Special Handling,” 

mark "Saturday delivery." (Do NOT 

mark "hold for Saturday")

Quality Control Samples* Equipment Blank Water Equipment Blank Sediment Duplicate Ambient Blank Matrix Spike (not oiled site)

TAL (Test 

America 

Laboratories), 

Pensacola, Fla. 

ALL 

CONTAINERS 

(EXCEPT "RA") 

ARE SUPPLIED 

BY TAL, PLUS 

ONE VOC TRIP 

BLANK AND ONE 

TEMPERATURE 

BLANK

250-mL poly, with 

H2SO4 for nutrients

(TKN, NH4, and TP)

Use precleaned, 

blanked 

1-L RA bottle to 

collect dip sample and 

fill acid-preserved 

250-mL brown poly 

bottle. Leave 

headspace. Check pH 

and add additional 

H2SO4 to pH < 2, if 

needed. Chill to 4oC 

without freezing.

CHILL to 4oC. Place 

in sealed plastic bag. 

Ship priority overnight, 

protected from 

meltwater and in a 

leakproof cooler.

850-471-6227

marty.edwards@testamericainc.com

Marty Edwards 

3355 Mclemore Drive 

Pensacola, FL 32514

√ √ √ √

*All containers are filled for routine environmental and triplicate samples. Up to one triplicate sample per Water Science Center may 

be collected at one site with a visible oil slick or sheen. One equipment blank for water and one equipment blank for sediment is to be 

processed by each Water Science Center. One duplicate sample for each site type (beach or marsh) is to be collected by each Water 

Science Center. One ambient blank is to be processed by each Water Science Center. One matrix spike sample should be processed 

by each Water Science Center for one beach and one marsh site that does not appear to have been impacted by oil. Refer to Section 6 

of the protocol for details on sample collection and processing; for detailed QA/QC sampling information, refer specifically to 

section 6.5.
135 

Table D-2. Post-landfall sediment samples: Laboratory, sample, shipping, and quality-control requirements.

LABORATORY

SEDIMENT-SAMPLE 

CONTAINER TYPE 

AND VOLUME -- 

ANALYSIS

COLLECTION and PRESERVATION 

Wipe all containers clean and dry, 

remove sediment from container 

and cap threads, check label, 

before packing.

SHIPPING 

Fedex Priority Overnight 

PROTECT SAMPLES FROM 

CONTACT WITH ICE 

MELTWATER: Double-bag and 

seal each sample using heavyduty ziplock bags and doublebag the ice (total of 4-bag layer 

between ice and containers). 

ENSURE THAT COOLERS ARE 

LEAK-PROOF.

SHIPPING ADDRESSES

NOTE SHIPPING INSTRUCTIONS AND 

CONTACTS FOR SATURDAY 

DELIVERIES.

Quality

Control 

Samples*

Equipment Rinsate 

Blank 

Duplicate

Triplicate

Dr. Amanda 

Demopoulos, 

Gainesville, Fla.

(Benthic Invertebrates)

Six 500-mL poly jar. 

Six sediment cores, 

each in a 500-mL

poly jar – Analysis: 

Benthic Invertebrates

Collect 6 sediment cores: 2-inch 

depth from surface; space cores 

approx. 1 m apart within 

sampling area. Extrude each core 

into a 500-mL jar. First 3 cores: 

fill to top with 10% formalin 

supersaturated with sodium 

borate and label jars "10% 

buffered formalin." Next 3 cores, 

no preservative. Seal lids with 

duct /electrical tape. CHILL.

CHILL to 4°C. Wrap sample 

jar in absorbent paper, put into 

double ziplock bags and seal. 

Tracking #’s to

ademopoulos@usgs.gov 

Note Saturday-delivery 

shipping address for 10/16.

Ship overnight or freeze and 

ship next day.

352-264-3490

ademopoulos@usgs.gov 

Dr. A. Demopoulos, USGS, 

Southeast Ecological Science Center, 

7920 NW 71st St., Gainesville, FL 

32653. Saturday 10/16 delivery: 

Ship to A. Demopoulos, 5010 NW 

64th Blvd., Gainesville FL 32653, 

352-346-6938

Dr. Robert Rosenbauer, 

Menlo Park, Calif.

Two 500-mL I-Chem 

or equivalent 

certified fired glass 

widemouth fired 

bottle (BGC) --

Analysis: Oil 

Fingerprint

Freeze samples. Fill no more than 

80% to allow room for expansion 

when frozen. Use a Kimwipe to 

dry jars and remove particles 

from threads and lid and cap 

tightly. Seal cap with electrical 

tape. KEEP JARS UPRIGHT. 

FREEZE. Keep samples 

chilled and ship frozen on dry 

ice asap. Place sample jars in 

foam or bubble sleeves and 

seal in zip-locks. KEEP JARS 

UPRIGHT. Saturday 

delivery: tracking #’s to 

tlorenson@usgs.gov; notify 

Tom Lorenson 650-642-5627

650-329-4198; 650-575-9965 (c)

brosenbauer@usgs.gov 

Dr. R. Rosenbauer, USGS, MS 999, 

345 Middlefield Rd, Menlo Park, CA 

94025. For Saturday 10/16/10 

delivery: Hold at FedEx Center 

3750 Haven Ave., Menlo Pk., CA 

94025 for pick-up by T. Lorenson

tlorenson@usgs.gov 650-642-5627

√ - √
136 

Table D-2. Post-landfall sediment samples: Laboratory, sample, shipping, and quality-control requirements.—Continued

LABORATORY

SEDIMENT-SAMPLE 

CONTAINER TYPE AND

VOLUME -- ANALYSIS

COLLECTION and 

PRESERVATION 

Wipe all containers clean and 

dry, remove sediment from 

container and cap threads, 

check label, before packing.

SHIPPING 

Fedex Priority Overnight 

PROTECT SAMPLES FROM 

CONTACT WITH ICE 

MELTWATER: Double-bag and 

seal each sample using heavyduty ziplock bags and doublebag the ice (total of 4-bag layer 

between ice and containers). 

ENSURE THAT COOLERS ARE 

LEAK-PROOF.

SHIPPING ADDRESS

NOTE SHIPPING INSTRUCTIONS 

AND CONTACTS FOR SATURDAY 

DELIVERIES. 

Quality Control 

Samples* Equipment Rinsate Blank Duplicate

Tiplicate

Dr Robert Rosenbauer, 

Menlo Park, Calif.

One 250-mL I-Chem or 

equivalent certified 

fired glass widemouth 

fired bottle (BGC) --

Analysis: Tar balls --

weathering 

characteristics

Collect tar balls wearing Teflon 

gloves, sized from thumbnails 

to palm-sized into 250 widemouth jar. CHILL to 4°C.

CHILL to 4°C. Place sample 

jar in foam or bubble sleeves 

and seal in ziplocks. KEEP 

JARS UPRIGHT. Saturday 

delivery: notify and send 

tracking #’s to 

brosenbauer@usgs.gov

650-329-4198

brosenbauer@usgs.gov

See Rosenbauer above for Sat. 

delivery information.

Dr. R. Rosenbauer, USGS, MS 

999, 345 Middlefield Rd, Menlo 

Park, CA 94025

Dr. Art Horowitz, 

Norcross, Ga.

One 18-oz (532-mL) or 

two 18-oz WhirlPak 

(see Collection) --

Analysis: Metals and 

trace elements; 

nutrients

Fill WhirlPak(s) from the bulk 

sample composite. Collect 1-kg 

in two 500-g WhirlPaks if 

sediment is sand-sized. If 

dominant grain-size consists of 

fines or mud, fill one 500-g 

WhirlPak. Keep in dark and 

chilled. 

DO NOT FREEZE.

CHILL, DO NOT FREEZE. 

Keep in dark and chilled at 

4°C. Double-bag. Saturday 

10/16/2010 delivery: (1) 

notify Kent Elrick & email 

him the FedEx tracking #’s/ 

kaelrick@usgs.gov

(2) Check Hold Sat. box on 

shipping label. (3) FedEx 

office: FedEx, 6650 Corners 

Industrial Ct., Norcross GA 

30092

770-903-9153

horowitz@usgs.gov

Saturday delivery (10/16/10) – 

note on address label Att: K. 

Elrick. FedEx to hold for Sat. 

pick up. Mon.– Thur. ship to:

A. Horowitz, Georgia Water 

Science Center, Peachtree 

Business Center, Suite 130, 3039

Amwiler Rd, Atlanta, GA 30360

- √
137 

Table D-2. Post-landfall sediment samples: Laboratory, sample, shipping, and quality-control requirements.—Continued

LABORATORY

SEDIMENT-SAMPLE 

CONTAINER TYPE AND

VOLUME -- ANALYSIS

COLLECTION and 

PRESERVATION Wipe all 

containers clean and dry, 

remove sediment from 

container and cap threads, 

check label, before packing.

SHIPPING 

Fedex Priority Overnight 

PROTECT SAMPLES FROM 

CONTACT WITH ICE 

MELTWATER: Double-bag 

and seal each sample using 

heavy-duty ziplock bags and 

double-bag the ice (total of 4-

bag layer between ice and 

containers). ENSURE THAT 

COOLERS ARE LEAKPROOF.

SHIPPING ADDRESSES

NOTE SHIPPING 

INSTRUCTIONS AND CONTACTS FOR 

SATURDAY DELIVERIES. 

Quality 

Control 

Samples* Equipment Blank Sediment Duplicate Triplicate

Dr. John Lisle, 

St. Petersburg, Fla.

18 oz. (532 ml) in 

double WhirlPak 

(For equipment blank 

only—place WhirlPak 

sample into a 

widemouth jar.

Analysis: 

Microorganisms

Use sterile equipment. Fill 

WhilPak from the bulk 

sample composite. FREEZE 

sample to -20°C.

FREEZE. Ship doublebagged sample overnight on

dry ice. Isolate samples 

from meltwater. NOTEsend tracking #s to J. Lisle 

jlisle@usgs.gov; use home

shipping address for 

Saturday deliveries.

727-803-8747 x3140 Office, 

jlisle@usgs.gov

Dr. J. Lisle, USGS, Center for Coastal 

Watershed Studies, 600 4th Street, So., 

St. Petersburg, FL 33701

For Saturday delivery, ship to: J. Lisle, 

2249 Hidden Meadows Dr., Palm 

Harbor FL 34683, 727-512-7805

√ - √

USGS Marine 

Ecotoxicology Research 

Station TAMU-Corpus 

Christi Center for 

Coastal Studies, Texas

Two 1-L clear or amber 

wide-mouth glass bottle 

(BGC) -- 

Analysis: Pore-water 

toxicity

Fill bottles to top from bulk 

sample. Use Kimwipe to 

remove particles from jar 

threads and lip, tightly close 

& seal cap, using electrical 

tape. KEEP JARS UPRIGHT

IN COOLER. 

CHILL at 4°C. DO NOT 

FREEZE. Place jars in 

bubble wrap, then into 

doubled ziplock bags; seal.

NOTE- send tracking #’s 

to james_biedenbach@usgs.gov

Ship to home address for 

Saturday deliveries.

361-825-3217 (Fax )361-825-3270

scott_carr@usgs.gov Dr. Scott Carr

james_biedenbach@usgs.gov

Dr. J. Biedenbach, USGS Marine 

Ecotoxicology Research Ctr 6300 Ocean 

Dr. NRC Suite3200, Unit 5867, Corpus

Christi, TX 78412. Saturday delivery:

James Biedenbach, 2121 Dorsey St., 

Corpus Christi TX 78414, 

361-331-7621

- √
138 

Table D-2. Post-landfall sediment samples: Laboratory, sample, shipping, and quality-control requirements.—Continued

LABORATORY

SEDIMENT-SAMPLE 

CONTAINER TYPE AND

VOLUME -- ANALYSIS

COLLECTION and 

PRESERVATION Wipe all 

containers clean and dry, 

remove sediment from 

container and cap threads, 

check label, before packing.

PROTECT SAMPLES FROM 

CONTACT WITH ICE 

MELTWATER: Double-bag,

seal each sample in heavyduty ziplock bags; doublebag ice (total of 4-bag layer 

between ice and containers). 

NO LEAKY COOLERS. 

SHIPPING ADDRESS Quality 

Control 

Samples* Equipment Rinsate Blank Duplicate Triplicate

Test America, 

Pensacola, Fla.

ALL CONTAINERS 

ARE SUPPLIED BY 

TAL, PLUS ONE 

TEMPERATURE 

BLANK

One 8-oz wide mouth 

jar -- Analysis: Oil & 

Grease HEM (Method 

1664A, CIN 50137), 

SVOC TCL (Method 

8270D; CIN 50117)

Fill from bulk sample 

composite. Use a Kimwipe to 

remove any particles from 

threads and lip, tightly seal 

cap. Double bag, chill to 4°C.

CHILL at 4°C. Wrap jar in 

bubble wrap, place into 

double-bagged ziplock bags

and seal. Ship overnight.

850-471-6227

marty.edwards@

testamericainc.com

Marty Edwards, 

3355 Mclemore Dr. 

Pensacola, FL 32514

√ √√

One 4-oz wide mouth 

jar -- Analysis: 

Alkylated PAH and 

PAH (Method 8270C 

SIM; CIN 50641)

Fill from bulk sample 

composite. Use a Kimwipe to 

remove any particles from 

threads and lip, tightly seal 

cap. Double bag, chill to 4°C.

CHILL at 4°C. Wrap jar in 

bubble wrap, place into 

double-bagged ziplock bags

and seal. Ship overnight.

√√

*All containers are filled for routine environmental and triplicate samples. One triplicate sample set per water science center may be 

collected at an oiled site. One equipment blank for sediment will be processed by each water science center. One duplicate sample for 

each site type (beach or marsh) is to be collected by each water science center. Refer to Section 7 of the protocol for details on 

sample collection and processing; for detailed QA/QC sampling information, refer specifically to sections 7.5 and 9.
139 

Appendix E. Health and Safety 

Appendix E–1. Health and Safety Plan Package

Appendix E–2. Job Hazard Analysis

 

Appendix E–3. USGS Safety Bulletin (7/21/2010): Personal Flotation Device 

Selection and Use

Appendix E–4. Contacts for Deepwater Horizon Incident Response (current as of 

8/6/2010)

Appendix E–5. Instructions for British Petroleum (BP) Site-Specific Training 
140 

Appendix E-1. Health and Safety Plan Package

USGS personnel working under the direction of the Incident Command or other Federal Agency 

are to follow that organization’s HASP. USGS HASP requirements for response to the Gulf of 

Mexico Deepwater Horizon oil spill are fulfilled by assembling a USGS DWH GOM HASP 

package, which should be kept on hand when deploying to the field site. This package includes 

the following documents (the following HASP elements also can be accessed through a 

www.my.usgs.gov wiki12):

1. Agency HASPs. A HASP provided by the Incident Command (IC) or Agency under 

whose jurisdiction the work will be conducted is required. In this case, the HASP 

provided by the U.S. Fish and Wildlife Service (FWS) will suffice, unless directed 

otherwise. 

a. U.S. Coast Guard (http://www.uscg.mil/forms/ics/ICS_208_CG.pdf), 

b. U.S. Fish and Wildlife Service 

(http://internal.usgs.gov/ops/safetynet/FWS%20WIldlife%20Branch%20HASP%20(M

C%20252%20Oil%20Spill).pdf)

2. The Daily Operational and Safety Situational Report (the “shift” or operations 

plan). The Shift Plan – which usually covers a 48-hour time period – is obtained from the 

designated IC safety or Industrial Hygiene staff on or for the day(s) of field deployment. 

Arrangements can be made to receive the Shift Plan via e-mail for the time period of 

planned field deployment to avoid delay of field work by contacting the USGS Bureau 

Industrial Hygienist (Anthony Zepeda, 703-648-7551), or by contacting: 

a. Houma LA Incident Command - 1697 Highway 311, Houma LA 70395, 

Main 985-493-7600; Operations 985-493-3343; mc252decon@gmail.com. 

b. Mobile AL Incident Command - One South Water Street Mobile AL 36602, 

251-442-1938. 

3. Evacuation Plan. The Evacuation Plan generally is separate from the Shift Plan. 

Evacuation plans are specific to and provided either by the Huoma, La., or Mobile, Ala.,

Incident Command Sectors, as appropriate. The field team should request the latest 

Evacuation Plan when requesting the Shift Plan and include it in their HASP package. 

Eamples are linked to the HASP Package of the my.usgs.gov wiki (see footnote #12). 

4. Job Hazard Analysis (JHA). A draft JHA for Houma GOM-DWH is included in 

Appendix E-2 and is linked on the HASP Package section of the wiki (footnote #12).

5. Section 3.0 of this Sampling Protocol. A copy of this section is linked on the HASP 

Package section of the my.usgs.wiki (see footnote #12).

 

12 These wiki files are readily accessible by USGS personnel; non-USGS personnel should contact the Office of 

Water Quality (703-648-6862 or 703-648-6866 or 703-648-6902 for access privileges): 

https://my.usgs.gov/josso/signon/login.do?josso_back_to=https://my.usgs.gov/OWQ_Deep_OilWiki/josso_security

_check
141 

Consideration should be given to supplementing the HASP with additional topical information to 

cover health, safety, and hazards conditions that may be unique to USGS sampling sites. For this 

purpose, the USGS Template HASP for Oil Impacted Areas was developed for use by USGS 

personnel: 

http://internal.usgs.gov/ops/safetynet/HASP%20for%20Oil%20Spill%20Impacted%20Areas.doc

Supplemental information can be found at http://1stop.usgs.gov/safety/topic/jha/index.html .
142 

Appendix E-2. Job Hazard Analysis

Job Hazard Analysis

• Check or highlight the numbered box(s) for all significant safety concerns this project should address. 

Significant safety concerns are commonly those that require training, purchase of safety equipment, or 

specialized preparation to address potentially hazardous conditions. 

• Identify any unlisted safety concerns at bottom of the page.

• Provide details on the back of this page.

Project Title (Short)____________________________________________________________

Field Team / Supervisor_________________________________________________________

Site ID and Date_______________________________________________________________

√ Safety Concerns

1. Wading, bridge, boat, or cableway measurements or sampling

2. Working on ice covered rivers or lakes

3. Measuring or sampling during floods

4. Well drilling; borehole logging

5. Electrical hazards in the work area

6. Construction

7. Working in remote areas, communication, office call in procedures

8. Ergonomics, carpal tunnel syndrome

9. Field Vehicles appropriate for task?- Safety screens, equipment restraints. 

10. All terrain vehicles, snowmobiles

11. Helicopter or fixed wing aircraft usage

12. Site access

13. Hypothermia or heat stroke

14. Hantavirus, Lyme Disease, Histoplasmosis, Pfiesteria, Others?

15. Contaminated water with sanitary, biological, or chemical concerns

16. Immunizations

17. Laboratory or mobile laboratory. Chemical hygiene plan.

18. Hazardous waste disposal

19. Hazardous waste site operations

20. Confined space

21. Radioactivity

22. Respiratory protection

23. Scuba Diving

24. Electrofishing

25. Use and disposal of chemical reagents

(Job Hazard Analysis continued on next page.)
143 

Box

no. 

For each numbered box checked on the previous page, briefly:

A. Describe the safety concern as it relates to this project. 

B. Describe how this safety concern will be addressed. Include training, safety 

equipment and other actions that will be required. 

C. Estimate costs.

1. Wading in Gulf of Mexico surf zone to 3 feet of water. 2 to 3-person team working at sampling 

location, each with USGS-approved PFD, waders, and PPE, as described in the USGS Gulf of 

Mexico Deepwater Horizon (GOM DWH) Sampling Protocol.

7. Remote sites may not have 911 access; precautions are taken to have on hand cell phones or 

radios and emergency contact numbers.

9. Field vehicles, including motorcraft, comply with DOI/USGS regulations and standards, include 

proper http://1stop.usgs.gov/safety/topic/jha/index.htmlsafety equipment, chemical spill kits, and 

MSDS sheets.

12. Access to hot zones is verified daily with the Coast Guard Incident Command. 

13. Summer conditions and PPE requirements could aggravate potential for hypothermia or heat 

stroke; HASP is on hand that details personnel behavior and work constraints when working 

under these conditions, including rest periods, liquid intake, and emergency procedures.

15. Potential exposure to crude oil products. HASP and GOM DWH Sampling Protocol dictate the 

PPE and safe sample-handling procedures. Minimum of 24 hours of HazWOper training is 

current and completed.

17. Mobile laboratory contains and conforms to the WSC chemical hygiene plan.

18. Oil-soiled disposable equipment and garments and cleaning solutions will be disposed in 

accordance with the OSHE and USGS protocols, as described in the USGS GOM DWH 

Sampling Protocol and in accordance with State and local regulations. 

19. Training has been completed for setting up and working in Hot (Exclusion) zones, Contamination 

Reduction Zones, Support Zones, and a Contaminant Corridor and is detailed in the USGS GOM 

DWH Sampling Protocol. Sampling and decontamination activities will be carried out using these 

procedures.

22. Potential exists for volatile hydrocarbon exposure to the respiratory system. The field team will 

follow the exposure-detection protocol, monitoring exposure levels using a PID while on site as 

directed in the USGS GOM DWH Sampling Protocol, evacuating the site at a PID measurement 

of 20 ppmv and 5 ppm for Benzene, and executing the evacuation procedures provided by 

Incident Command and informing the Industrial Hygienist (IH) on duty of the evacuation. Field 

personnel will not return to the site until it is cleared by the IH and will not be working under 

conditions that require use of a respirator.

25. Potential contact with chemical sample preservatives: Formalin, sulfuric acid, nitric acid, and 

hydrochloric acid. The specific JHAs for these substances are included in this HASP and field 

personnel have been briefed regarding the hazards and proper use and handling of these chemical 

substances.

 

Discussed job hazard analysis (JHA) with Water Science Center’s 

• Collateral Duty Safety Officer Yes____ No____

• Copy of JHA given to Collateral Duty Safety Officer Yes____ No____

Water Science Center Director/Supervisor ___________________ Date ___________

Regional Program Officer _____________________________________ Date ___________

(Job Hazard Analysis continued on next page.)
144 

Appendix E-2. Job Hazard Analysis.—Continued

Job Hazard Analysis Plan for (Project Title): 

Instructions for Employees: 

Each employee shall comply with occupational safety and health standards and all rules, 

regulations, and orders issued pursuant to this project, which are applicable to his or her own 

actions and conduct. Management is responsible to ensure that all safety policies are 

implemented and monitored at the field level. Supervisors must ensure that employees are 

informed of safety policies; that the policies are integrated into field operations; and that they are 

carried out in a proper and consistent manner. However, once you have received training and 

have been assigned an activity, most of the responsibility for personal safety and that of others is 

yours. Your first responsibility is to think for yourself. Both supervisors and employees will be 

held accountable if safety policies are not followed. 

Preparing for the Field

In preparing yourself, consider the following elements. Many of the tasks assigned to USGS 

employees require strenuous exercise, sometimes under adverse weather conditions. 

Adequate planning for field assignments includes: Discussing the assignment thoroughly with 

your supervisor to ensure that you understand what is expected, why it needs to be done, and 

how it should be accomplished. Know where the nearest emergency medical facilities are 

located; make plans on how to contact these facilities if you are alone and severely injured 

(cellular phone). Reviewing maps, property descriptions, and notes made by yourself and others 

on previous visits to ensure that you are aware of site conditions and potential hazards that may 

exist. Contacting landowners and public officials to inform them of your plans and receive 

permission for access. Appropriate personal gear may include: Adequate clothing for weather 

conditions. Proper footgear that you will need for fieldwork, including hiking boots, steel-toed 

safety shoes, hip boots, hardhats, and waders. A PFD is required when working on boats and or 

while wading into the surf zone and wetland or marsh areas (see PFD Safety Bulletin dated 

7/21/2010). 

A list of required tools, instruments, and supplies should be made when planning your trip and 

these items should be checked to ensure they are in good operating condition before you start 

your trip (these are listed in Appendix B of the USGS GOM-DWH Sampling Protocol 

(https://my.usgs.gov/OWQ_Deep_OilWiki/). An office Call-in policy will be in effect for all 

field activities. Field personnel engaged in response to the Deepwater Horizon oil spill must 

obtain the daily or 48-hour Operational Plan (Shift Plan) before deploying to the field 

site, either from the USGS Bureau or Eastern Region Industrial Hygienist 

(A. Zepeda, 703-648-7551; B. Demith, 703-648-4636) or from the Houma Sector Unified 

Command FWS Safety Officer (Jack Morrow, 404-408-7226, john_morrow@fws.gov). 

We cannot eliminate all the hazards associated with our jobs. We can, however, reduce these 

hazards to reasonable risks. The intent of Job Hazard Analyses (JHAs) is to identify the hazards 

associated with our jobs and then develop realistic actions that can be used to reduce these 

hazards to reasonable workplace risks. 
145 

Additional JHA information for task-specific work is available on the WRD Safety Homepage 

http://1stop.usgs.gov/safety/topic/jha/index.html. 

Sampling in the Gulf of Mexico

Detailed instructions are provided in the USGS Sampling Protocol for Post-Landfall Deepwater 

Horizon Oil Release, Gulf of Mexico, 2010: Addendum to Standard USGS Methods for the 

Collection of Water, Sediment, Benthic Invertebrates, and Microorganisms (Sampling Protocol) 

and in the updated information posted in the OWQ_Deep_Oil Wiki, previously referenced. Field 

personnel must become familiar with the contents of the Sampling Protocol and abide by all the 

health and safety requires described, including the mandatory HazWOper and other training, 

PPE, and air-monitoring requirements, and are to check the wiki for bulletins and updates that 

affect personnel health, safety, and ability to perform their duties. 

Sampling and Measurements by Wading

Personal Flotation Devices (PFD's) are required in all operations near, in, or over water except in 

those cases where an approved site-specific Job Hazard Analysis (JHA) defines the conditions 

for an exemption (refer to the U.S. GEOLOGICAL SURVEY (USGS) SAFETY BULLETIN:

Personal Flotation Device (PFD) Selection/Use, issued 7/21/2010). In areas of potential 

contamination appropriate PPE must be worn, as described in the Sampling Protocol referenced 

above. Prevent water from contacting your skin. 

Floods

Rain can fall at a rate of several inches per hour and rapidly create dangerous conditions in the 

area where you are working. Weather forecasts, evacuation plans, and the daily briefing provided 

by the local Incident Command are necessary in planning activities to ensure your safety. 

Maintain an updated copy of your floodplan. Maintain regular office and IC contact during 

emergency conditions. Have the proper rescue equipment on hand and use it according to your 

plan. Make sure you have emergency communication capability in case of an accident. Raingear 

must meet color requirements of the state and reflective requirements of ANSI Class III 

garments. 

Remote Areas, Communications

Mobile telephones provide a minimum precaution. Satellite communication services might be 

available for remote areas where cellular service is not available. Make an itinerary for every 

field trip and leave a copy at the office and with the IC in addition to family or colleagues. 

Schedule times to check in at work and with family or colleagues when field trips require 

overnight stays. Follow the established schedule. Notify all concerned parties if your schedule 

changes. Obtain or reserve communication equipment, such as a cellular phone or two-way 

radio. It’s a good idea for all field crews to be aware of any potential medical conditions or 

treatments for existing medical conditions of the field-team members. Examples of these 

conditions would include severe allergic reactions, Diabetes, coronary problems, heat stress, etc. 
146 

Ergonomics 

Work-related musculoskeletal disorders (MSD) result when there is a mismatch between the 

physical capacity of workers and the demands of the job. Many of these are caused or aggravated 

by work related stressors such as such as lifting, reaching, pulling, pushing, and bending. Get 

assistance in moving heavy or large items to reduce back injuries. 

Field Vehicles

It is required that the installation of barriers behind the front seats of all vehicles that are used to 

carry heavy equipment is enforced. Defensive driver training will be given to all employees who 

are expected to operate motor vehicles on the job. All weights, compressed gas cylinders, and all 

other heavy or large items shall be appropriately secured in the vehicle. Gasoline, methanol, and 

other hazardous materials should be transported in leak proof containers (safety can) and secured 

to prevent movement and transported to prevent release of fumes. For all vehicles used in field 

situations, an appropriate fire extinguisher shall be securely mounted and easily accessible. 

Vehicle maintenance and condition are the responsibility of the users. 

Field Vehicles Must Have The Following Safety Equipment: 

Fire extinguisher, First Aid kit, PFD’s, PID, ANSI Traffic vests, Hardhat, Safety Glasses, Gloves 

(leather, cloth, chemical resistant), Traffic control lights, cones, emergency signs. 

Site Access 

Working in and around the surf zone and wetlands or marshes will subject you to conditions that 

can cause slips, falls, contact with contaminated water and sediments, impede mobility, and that 

could result in serious injury to you and your coworkers. You can't avoid all potential dangers, 

but you can minimize the risk of accidents by considering the following guidelines. 

1. Avoid steep slopes and navigate slippery conditions with care, using the buddy system. 

2. Do not enter the surf zone under rough surf conditions. 

3. When navigating through deep marsh muds, keep moving to avoid sinking into the muck and 

becoming immobilized. 

4. Adhere to PFD, PPE, and all other safety requirements. 

5. Be alert to significant wildlife threats, such as the potential to encounter alligators, snakes, or 

other domestic and wild animals and be prepared to take appropriate preventive and 

defensive action (National Field Manual for the Collection of Water-Quality Data, Chapter 

9). Biting insects, such as mosquitoes, chiggers, ticks, and various flies, are generally of less 

immediate hazard than stinging insects, but they may be carriers of disease. 

Dealing With Hostile Persons 

Be aware of radical or strong political groups operating in the area. Familiarize yourself with any 

controversial issues or illegal activities in the area you will be working. Be able to briefly explain 

the necessity for the data collection you are charged with. Formulate a plan for dealing with 

hostile people that includes avoidance or calm, deliberate departure from their presence. 
147 

Hyperthermia

Hyperthermia is a condition of increased body temperature caused by exposure to 

excessive heat. Contributing factors are physical exertion, clothing, humidity, lack of air 

movement, and temperature, but the most important factor is body hydration. The normal body 

requirement for fluids in temperate regions is 2 1/2 quarts per day; GOM conditions will require 

more fluid. Early warning symptoms of Hyperthermia are chilling, a throbbing pressure in the 

head, unsteadiness, dizziness, nausea, dry skin (either hot and red or cool and pale), rapid pulse, 

and muscle pains and spasms. 

Viral and Bacterial Issues 

USGS policy on respiratory protection and provides generic guidelines to assist centers in 

development of a safety program for employees who work in an environment with potential 

exposure to respiratory hazards. Respirators may not be used without appropriate medical 

surveillance and clearance. 

USGS personnel should assume that any water they sample, measure or gage may be 

contaminated with pathogenic organisms. It should be a regular practice after sampling to 

thoroughly disinfect with a biocidal agent (for example, germicidal soap or alcohol based 

cleaners) any exposed skin that has come in contact with the water.

Contaminated Water and Soil - Sampling Wastewater Disposal

Wear appropriate gloves and eye protection. Prevent water from contacting your skin. 

Appropriate immunizations are made available on a voluntary basis. Carry appropriate 

disinfecting solutions for cleaning of hands, equipment and materials. Calibration standards, 

decontamination and other cleaning solutions, and chemical preservatives must be handled and 

disposed of with respect to local environmental policies. Process samples with care. Always use 

appropriate gloves and safety glasses when handling samples and preservatives. Biohazards must 

be appropriately labeled, stored and disposed according to local regulations. 

Labs and Mobile Labs

Each USGS vehicle performing water quality work is considered a mobile lab. Mobile labs must 

meet the requirements of chemical transportation regulations of the DOT. Each vehicle will be 

supplied with a copy of the district chemical hygiene plan, Material Data Safety Sheets (MSDS) 

for any chemical carried and supplied with appropriate personal protective equipment. Any 

USGS personnel using chemicals shall be appropriately trained through lab safety, hazard 

communications training. Normally it is not necessary for USGS vehicles to be placarded. 

Mobile labs, including water-quality vehicles will meet the same standards of facility labs. 

Each vehicle will be supplied with chemical hygiene plans, MSDS’s, PPE, emergency eye 

wash, JHA’s appropriate to job tasks. 

Formalin and Formaldehyde

Formalin is a teratogen, which can cause adverse birth and reproductive effects. It is also a 

mutagen, which can cause DNA damage. If exposure exceeds 0.75 ppm for 8 hours (TWA) and 

greater than 2.0 ppm for and 15 minute period; all provisions listed in 29 CFR 1910.1048 shall 

apply. Wear appropriate gloves or clothing to prevent exposure. Wear safety goggles. Keep 
148 

formalin from contact with alkalis, acids, and phenols. Formalin or formalin-preserved samples 

will not be transported in the passenger compartments of vehicles. Wash thoroughly after 

handling formalin. http://1stop.usgs.gov/safety/topic/jha/formalin.html 

Dry Ice

Dry ice will be used to preserve specific samples for the GOM-DWH project and must be 

handled in accordance with the dry-ice JHA: http://1stop.usgs.gov/safety/topic/jha/DryIce.pdf

Acid Sample Preservatives

Some samples will be preserved with nitric (HNO3), hydrochloric (HCl), or sulfuric (H2SO4) 

acid, which must be handled as stipulated in the following JHAs: 

• HNO3 and HCl: http://1stop.usgs.gov/safety/topic/jha/acid_hcl_hno3.html

• H2SO4: http://1stop.usgs.gov/safety/topic/jha/acid_h2s04_amps.html

Decontamination Agents 

Chemical substances used for equipment cleaning and decontamination may include methanol 

(MeOH) and nitric or hydrochloric acids. The ASR referenced above for nitric and hydrochloric 

acid applies to the use of these chemicals as cleaning agents.

• MeOH: http://1stop.usgs.gov/safety/topic/jha/methanol.htm

Sampling in Weather Extremes

Fieldwork often is necessary under adverse atmospheric and other environmental conditions. 

Prepare for extreme conditions that might be experienced in your area of the country. Before 

leaving for the field, check the weather forecast using one or more of these options: the local 

television station, the national weather channel, the local land/marine weather band channel that 

constantly repeats current and future weather conditions, or computer networks. Extremes of air 

temperature occur in all parts of the country. The ideal comfort range for humans is between 16 

to 32oC (60 to 90oF). Hypothermia and Hyperthermia normally occur in temperatures outside this 

range.

Do nothing that will endanger the public. Use vehicle light bar (flashing lights), consult traffic 

control plan, and wear PFD or reflective vest. Do not park on bridge unless known to be safe. Do 

not attempt a wading measurement if there is any doubt that you will be able to safely cross the 

stream. 
149 

Personal Protective Equipment (PPE) as Required and Applicable

Field Work 

Personal Flotation Device (PFD) 

Hard Hat

Safety Glasses

Gloves (Work and Chemical Resistant)

Hip Or Chest Waders With or Without Steeltoes & Shanks 

Steel Toed Boots 

Cell Phone 

Reflective Clothing

Bridge And Traffic Safety Plan and Equipment 

Trip Plan

Boating 

PFD

USCG Required Equipment 

Trip/Float Plan

Water Quality

PFD

Antibacterial Cleaners

Safety Glasses

Gloves (Chemical)

Ground Fault Interuptors (GFI) for Use With AC Pumps 

Immunizations

Construction 

PFD

Hard Hat

Steel-Toed Shoes or Boots

Safety Glasses

Gloves 

Hearing Protection

Climbing Harness

Ground Fault Interuptors (GFIi) for Use With Power Tools 
150 

Appendix E-3. USGS Safety Bulletin (7/21/2010): Personal Flotation Device Selection 

and Use

U.S. GEOLOGICAL SURVEY (USGS) 

SAFETY BULLETIN: 

Personal Flotation Device (PFD) Selection/Use

DATE ISSUED: 

 07/21/10 

PAGE:

1 of 3 

AREA AFFECTED:

Gulf of Mexico (GOM) 

Deepwater Horizon Oil Spill 

Response/Cleanup Areas

OPERATIONAL PERIOD:

Remains in effect for the duration of USGS 

GOM Deepwater Horizon Oil Spill 

Activities or until superseded by 

supplemental guidance 

issued after 7/21/2010.

This Safety Bulletin provides clarifying information regarding Personal Flotation Device (PFD) 

use by U. S. Geological Survey personnel working within the Gulf of Mexico (GOM) Deepwater 

Horizon Oil Spill affected areas. This message is provided to answer specific questions raised by 

USGS employees regarding Agency requirements for PFD’s. It does not address aviation related 

PFD use requirements.

Agency personnel must comply with USGS PFD policy requirements [e.g. 445-2-H, Chapter 31, 

31.4 (A) (6)] and adhere to any supplemental Agency requirements established in response to 

GOM Deepwater Oil Spill watercraft related activities. USGS employees responding to any 

affected GOM area involving watercraft will provide their own PFD according to USGS Policy 

and supplemental information contained herein. If you are responding to any GOM affected area 

and do not have a PFD, contact your immediate supervisor and make arrangements to acquire 

one PRIOR to assignment or mobilization. If USGS employees are assigned to a Vessel of 

Opportunity (VOO), you are required to wear your own PFD, meeting Agency PFD 

requirements unless the VOO Operator mandates otherwise. (An example of this would be 

during extreme weather conditions or working on open decks of larger vessels where the VOO 

Operator provides a higher level of PFD safety.)

Question 1: Are personnel required to wear a PFD while on-board USGS, Partner, 

Agency, BP VOO, or any other GOM spill assigned watercraft? 

Yes. Although there are some exceptions provided in USCG, DOI and USGS policies, all 

personnel working aboard GOM Oil Spill assigned watercraft are required to wear a PFD. Such 

exceptions are typically based on vessel size/class and/or location of personnel on vessel (e.g., on 

the deck, in enclosed cabin areas, and at the discretion of the watercraft operator at other 

locations on the vessel. In regards to these exceptions, personnel must follow USGS 

Watercraft/PFD Policy requirements. USGS employees assigned to VOO Vessels are directed to 

provide and wear USGS approved PFD’s while on-board. In the event of extenuating 

circumstances, (such as severe weather or working on open decks of larger vessels), VOO 

Operators may provide crew with higher levels of safety such as a Type I PFD. In that case, 

USGS employees are directed to adhere to the VOO Operator mandates.
151 

Question 2: Are there any other specific times or activities when I need to wear a PFD? 

Yes. Numerous water based activities may be conducted during our work on the GOM Oil Spill 

and USGS employees must mitigate the hazard of drowning by wearing a PFD while working 

AROUND THE WATER (e.g., conducting work along shorelines), ABOVE THE WATER 

(e.g., on watercraft, structures or bridges), and NEAR THE WATER (e.g., wading). You and 

your Spill Supervisor must evaluate the hazards of any proposed work to ensure that adequate 

hazard mitigation measures have been implemented. Assistance in evaluating hazards can be 

gained by contacting your respective spill safety officer, local collateral duty safety coordinator 

or Bureau Watercraft Safety Program Manager.

CAUTION: NO PFD SHALL BE WORN UNDER ANY TYPE OF OUTER CLOTHING. 

Wearing any PFD under a Tyvek suit or under other layers of clothing may compromise 

the flotation of the PFD as well as increase the element of heat stress. 

Question 3: Is there a requirement for vessels to have a throwable device on-board a USGS 

watercraft? 

Yes. Any vessel 16 feet and greater (except canoes and kayaks) working the GOM Oil Spill, 

must carry one throwable Type IV device, (e.g., throw rings, cushions) (* throw-rope bags alone 

are not a Type IV) ready for immediate deployment. USGS Watercraft Operators and VOO 

Operators must indicate the throwable device location during a safety briefing before initial 

vessel departure.

Question 4: Must a PFD be U. S. Coast Guard approved? 

Yes. Approved PFD’s have an USCG approval number typically provided on the inside shell 

fabric or material. ALL PFD’s used on watercraft for the GOM Oil Spill must have the USCG 

approval. 

Question 5: What does “in good, serviceable condition” really mean? 

According to USGS Policy, PFD’s must be regularly inspected by the wearer to ensure the unit is 

in good, serviceable condition. All DOI-USGS PFD’s shall be International Orange (or ANSI 

Hi-Vis Lime-Green) in color). All adjustment straps, buckles and/or zippers should be in good 

working order. All outer shell and inner shell fabric should be intact without compromise. 

Approved, retro reflective tape should be intact and securely attached. PFD’s that are UV 

Damaged and faded in color should be immediately replaced. PFD’s with frayed or broken 

straps, broken zippers or buckles should be immediately replaced. PFD’s with cracked, faded or 

torn retro reflective tape should be immediately replaced. Any torn fabric (inner or outer shell) 

indicates a need for immediate replacement. All of the above inconsistent findings reference a 

PFD that is NOT in good, serviceable condition. 

Question 6: Are there different types of PFD’s? 

Yes. There are five (5) types of PFD’s which provide one of three forms of flotation. The five 

types include (1) Type I Off-Shore Life Jacket; (2) Type II Near-shore Buoyant Vest; (3) Type 

III Flotation Aid; (4) Type IV Throwable Device; and (6) Type V Special Use Device. BP 

requires VOO operators to furnish Type III PFD’s to VOO passengers that do not have a PFD. 

In all cases, each USGS employee will provide their own individual PFD before embarking upon 
152 

a VOO vessel. VOO Operators have the final authority to mandate wearing a VOO supplied 

PFD.

Question 7: Are there different sizes of PFD’s and is it important to match the size to the 

wearer? 

Yes. Many PFD types come in ranges of sizes from small to XXXL. Depending upon the 

manufacturer, (e.g., Stearns, Revere, Mustang Survival, etc.) the PFD may have side adjustments 

for dual sizing. Personnel who wear undersized PFD’s tend not to wear the unit correctly 

(unzipped and/or unlatched) which could lead to displacement from the wearer when water entry 

is made. A PFD that is too large for the wearer may come off upon water entry. USGS 

employees required to wear Tyvek style suits should ensure that their PFD fits properly over this 

outerwear.

Question 8: Where and how do I get a PFD when I’ve been assigned GOM Oil Spill related 

tasks involving watercraft operation or water hazards? 

If you are mobilized to a known area where there is NO OIL or NO OIL RESIDUE reported, you 

can use the standard USGS approved PFD that you have been supplied with. *note sizing 

requirements referenced in Question 7. 

If you are mobilized to an area where OIL and/or OIL RESIDUE has been reported or is 

suspected, USGS employees should consider the following guidelines: 

1. Oil and/or Oil residue, once attached to the fabric material of any standard PFD, likely 

cannot be removed from the fabric by conventional cleaning methods, thus rendering the 

PFD contaminated. Once the fabric is contaminated, the PFD will be deemed in 

“unserviceable condition” and must be disposed of properly. OIL and/or OIL residue 

contaminated PFD’s shall not reused, if contamination takes place. 

2. USGS employees shall consider the following options for USGS Approved PFD’s in 

areas of GOM OIL and/OIL Residue response:

a. West Marine/Port Supply is a common USGS vendor that offers a Type V PFD 

designed for the Oil Worker Profession. The flotation foam panels are dipped in a 

rubberized coating allowing it to be cleaned easily. This is a Revere Model 280 RT 

Work Vest with nylon straps and nylon buckles. Oil and/or Oil residue can easily be 

cleaned with mild soap and water or alcohol swabs. 

b. West Marine/Port Supply Product number is Model # 10967776. Special USGS 

pricing for this Work Vest (single or multiple vest purchase) is $30.00 each. 

c. The Revere Model 280 RT is manufactured with SOLAS Retro-Reflective Tape that 

DOES NOT meet the DOI Standards for necessary square inches of tape and MUST 

be modified in order to meet our Standards. 

• Pre-Cut patches of SOLAS (adhesive backed) Reflective Tape will be available 

from the Bureau Watercraft Safety Program Manager along with a detailed 

drawing of where the wearer shall attach the tape in order for the PFD to meet 

compliance standards. 
• It shall be the responsibility of the USGS employee to immediately notify the 

USGS Spill Supervisor upon modification of this PFD and the USGS Spill 

Supervisor will maintain records indicating the employee’s name and date of 

modification and Spill Supervisor’s name. 

• Revere Work Vest Model 280 RT PFD’s that are not modified accordingly 

SHALL NOT be used at any time for any water related USGS activities inside the 

GOM Oil Spill Area or during any watercraft activities outside the GOM Oil Spill 

area.

• Revere Work Vest PFD’s, once modified, may be used in other watercraft 

activities outside the GOM Oil Spill areas. 

INFLATABLE PFD’s:

NOTE: According to USGS Policy, with any inflatable PFD, the wearer MUST conduct minimal 

semi-annual oral inflation tests, allowing the unit to stand, inflated, for a 24 hour period. 

Traditional, automatic inflatable PFD’s (wafer style) must be annually inflated by submerging in 

water, leak testing, drying and re-arming. Newer MUSTANG HAMMER (hydrostatic) 

INFLATOR MECHANISMS are allowed to go 4 years before automatic inflation is required 

(new USGS Policy). IN ALL CASES, the periodic testing of inflatable PFD’s are to be recorded 

in a “maintenance log” maintained by the wearer and a copy sent to the local CDSPC of the 

Cost Center. During any Center Safety Audit/Inspection, these maintenance records are to be 

made readily available to the person(s) conducting the audit/inspection. Failure to comply with 

this USGS maintenance requirement may result in the wearer forfeiting the continued use of the 

inflatable PFD.

USGS Policy further states that employees opting to wear any inflatable PFD must undergo 

documented training exercises before wearing this PFD as a primary device.

 Prepared by: Gary L. Hill, USGS Watercraft Safety Program Manager, (727) 803-8747 ext 3004

153 

 
154 

Appendix E-4. Contacts for Deepwater Horizon Incident Response (current as of 

8.06.2010)

Unified and/or Incident Command Specific to Deepwater Horizon Response 

• Houma LA Incident Command - 1697 Highway 311, Houma LA 70395, 

Main 985-493-7600; Operations 985-493-3343; mc252decon@gmail.com

• Mobile AL Incident Command - One South Water Street Mobile AL 36602, 251-442-

1938. 

• Houma Sector, Wildlife Branch Safety Officer -- BP persistent cell phone (985-665-

7093) 

• BP-provided persistent phone for Houma Safety Officer (Glen Stapleton) 985-709 

5957 

• St. Petersburg FL Incident Command – Fish and Wildlife Research Institute, 100 8th 

Avenue SE, St. Petersburg FL 33701, 904-755-8008

• Fish and Wildlife Service (FWS) Safety Officer, Mobile, AL - Gary Wilson, 

Gary_Wilson@fws.gov, 503-803-0888; or Brian_Hardison@fws.gov 404-376-3035 

• Fish and Wildlife Service Safety Officer, Houma, LA - Jack Morrow 985-665-7093 

(Unified Command) or 404-408-7226, John_Morrow@fws.gov 

• DOI Occupational Safety and Health Manager - Barry Noll, barry_noll@ios.doi.gov, 

Cell: 202-288-6843 

Safety Contacts Specific to Deepwater Horizon Response 

USGS personnel should contact the Safety point of contacts to obtain current guidance on safety 

and health issues such as known hazardous conditions. Your local and Regional USGS Safety 

and Health staff should be able to provide assistance if primary points of contact are not 

available. Jack Marrow, Fish and Wildlife Service (FWS) Safety Officer, Houma Sector, at 985-

665-7093. 

• Gary Wilson, Fish and Wildlife Service (FWS) Safety Officer, Mobile Sector, at 503-803-

0888. 

• Tim Radtke, DOI Industrial Hygienist, 303-638-2623 

• Regional Safety Office, if the above are not available

PFD and other Watercraft Safety Issues Specific to Deepwater Horizon Response

• Gary L. Hill, Bureau Watercraft Safety Program Manager, USGS Center for Coastal and 

Wetland Studies, St. Petersburg FL: 727-803-8747 (land)/ 727-365-0070 (cell); 

garylhill@usgs.gov. 
Online safety and health resources/information Specific to Deepwater Horizon Response

• Joint Incident Command: 

http://www.deepwaterhorizonresponse.com/go/doctype/2931/53023

• DOI: http://www.doi.gov/deepwaterhorizon/, and 

https://www.smis.doi.gov/smisaux/OilSpillInfo.htm

• USGS: http://www.usgs.gov/deepwater_horizon/, and 

http://internalgov/ops/safetynet/oilspillworkers.html

Waste Disposal and Other Environmental Issues Specific to Deepwater Horizon Response

Waste disposal and other environmental issues should be referred to the following DOI IC staff: 

• Doug Mutter, PMB/OEPC - Douglas_Mutter@ios.doi.gov 

• Stephen Spencer, PMB/OEPC - Stephen_Spencer@ios.doi.gov Cell: 505-249-2462 

Watercraft Decontamination Specific to Deepwater Horizon Response

USGS personnel should notify the IC regarding decontamination services for WSC vessels. 

• Mobile IC Decon Center: 985-493-3343, or mc252decon@gmail.com, or Mobile Decon 

Center 251-455-3010 (for locations of Mobile IC Regon Decon Centers, see 

http://www.bpdecon.com).

Use of Vessels of Opportunity (VOO) Specific to Deepwater Horizon Response

• VOO coordination hotline: 866-279-7983 or 877-847-7470 

• Vince Mitchell, VOO Program Coordinator for Houma, LA, 427-773-9983. 

Air Monitoring Specific to Deepwater Horizon Response

• Bob Garbe (DOI Occupational Health Program Manager): Robert_Garbe@ios.doi.gov, 

303-810-9934 (cell) 

• Tim Radtke (DI Industrial Hygienist: Tim_Radtke@ios.doi.gov, 303-638-2623 (cell) 

• Houma, LA Incident Command Center (Main Office): 985-493-7600 

• Anthony Zepeda USGS Bureau Industrial Hygienist: – azepeda@usgs.gov, 703-648-7551. 

E-mail or fax (703-648-7592) copies of field form with PID readings. 

• Beth Demith, USGS Eastern Region Industrial Hygienist: bdemith@usgs.gov, 703-648-

4636 

Air–monitoring results specific to the Deepwater Horizon response can be found under the 

following URLs: 

• USEPA - http://www.epa.gov/bpspill/air.html

• Current Air Quality along the Gulf Coast - http://gulfcoast.airnowtech.org/

155 
156 

Accident Reporting

All USGS accidents shall be reported within the DOI Safety Management Information System 

(SMIS) accessible at https://www.smis.doi.gov/ and clicking on "Accident Reporting" tab. Note 

that under the "Special (Disaster Response Related) Accident Report" selection, the department 

has added the following category "During the Response to the Gulf Oil Spill." Please mark this 

category when reporting accidents involving individuals who become ill or are injured during 

natural disaster relief efforts. On the injury selection page there is an entry button that allows the 

reporting supervisor to categorize an injury due to the Department’s response. This specialized 

entry page has specific questions on PPE and training. Questions related to SMIS may be 

directed to the DOI Occupational Safety and Health Manager, 202-288-5549/202-904-0008 or 

USGS HQ Safety and Health Specialist 703-648-7553. 
157 

Appendix. E-5. Instructions for British Petroleum (BP) Site-Specific Training 
158 

Appendix F. Examples of a Field Form and Analytical Services Request 

and Chain of Custody Forms Specific to USGS Sampling in Response to 

the Deepwater Horizon Oil Spill

Appendix F-1. Field Form for DWH Oil-Release Sampling (4 pages)

 

Appendix F-2 Examples of Analytical Services Request (ASR) and Chain-of-Custody 

(CoC) Record Forms 
159 

Appendix. F-1. Field Form for DWH Oil-Release Sampling 
160 
161 
162 
163 

Appendix. F-2. Examples of Analytical Services Request and Chain of Custody

Forms

F-2A ASR-CoC for Sediment Analyses by TestAmerica Laboratory

F-2B ASR-CoC for Water Analyses by TestAmerica Laboratory

F-2C ASR-CoC for Replicate Sediment Analyses by TestAmerica Laboratory

F-2D ASR-CoC for Blank Water Analyses by TestAmerica Laboratory
164 

Appendix. F-2A. ASR-CoC for Sediment Analyses by TestAmerica Laboratory 
165 

Appendix F-2B. ASR-CoC for Water Analyses by TestAmerica Laboratory
166 

Appendix F-2C ASR-CoC for Replicate Sediment Analyses by TestAmerica Laboratory
167 

Appendix F-2D ASR-CoC for Blank Water Analyses by TestAmerica Laboratory
168 

Appendix G. Manufacturer Guidance for Use of Multiparameter Sondes 

in Oil-Contaminated Waters

Attachment 1. YSI, Inc.: Cleaning, Care, and Deployment of Multiparameter Sondes 

and Sensors (Published with permission.) (6 pages)

 

Attachment 2. IN-SITU, Inc.: Cleaning and Care of Multiparameter Sondes and 

Sensors (4 pages) 
169 

Attachment 1. YSI, Inc.: Cleaning, Care, and Deployment of Multiparameter Sondes 

and Sensors (Published with permission.) 

Recommended Procedures for Use of YSI Water Quality Monitoring 

Instruments during Oil Spills 

Overview: This is a guidance document that is intended for users of YSI 6‐Series sondes and 

handheld instruments in environments impacted by an oil spill. The specific form and impacts of oil 

in water on YSI’s equipment can vary. These guidelines are our best practices for decontaminating 

and deploying equipment; however, they do not guarantee that sensors or equipment will not be 

impacted by the oil. 

YSI encourages customers to continue to collect data during an oil spill. We ask 

all users who are working in oil‐impacted areas to provide us with feedback on sensor 

performance and oil conditions, so that we can improve this document. Please send any 

information to environmental@ysi.com. 

For the 2010 Gulf of Mexico oil spill, we will guarantee expedited (3‐5 working days) 

repairs on equipment affected by the oil at our Ohio and Baton Rouge (USA) repair facilities. 

Instrument Decontamination 

If you have YSI instruments that are contaminated with crude oil, follow this 

decontamination procedure. 

You will need: 

• Gloves 

• Eye protection (safety glasses with side shields; or goggles) 

• Cloths or lint free paper towels 

• Replacement brushes and wipers and hex wrench 

• Dawn dishwashing liquid and Simple Green (degreasing formula) 

• Buckets 

• Soft brushes for cleaning 
170 

• Pipe cleaners and Q‐Tips 

• Waste collection container 

Procedure: 

1. Wear gloves and eye protection when handling items contaminated with crude oil. 

2. Spray all contaminated areas with Simple Green to remove as much contaminant as 

possible. 

3. Use soft cloth or paper towels to wipe off excess oil from instruments and sensors. 

 Be careful when wiping around sensor optics or membranes. 

 Dispose of oil‐saturated cloths according to local regulations (see note below). 

4. Remove oil‐coated wipers and brushes from sensors. 

5. Submerge instrument in warm, soapy water. 

6. Use soft brush to wipe away remaining oil. 

7. Use small brush to clean inside the conductivity cell of the temperature‐conductivity 

probe. 

8. Rinse in soapy water. 

9. Repeat steps 4‐7, several times if necessary. Dispose of oily water according to local 

regulations for hazardous materials (see note below). 

10. Do a final rinse in a fresh container of warm soapy water followed by a rinse in clean water. 

11. Dry and install new wipers and brushes. 

Oil Effects on Specific Water Quality Sensors 

The most common problems with sensors will be related to sensors having been in 

contact with oil. Special attention should be paid to the following sensors in the decontamination 

and calibration steps. 

1. pH: The performance of the pH and pH/ORP sensors due to the sensitivity of the glass 

bulb and reference junction. The pH sensor may require additional cleaning steps and 

may benefit from elevating the soapy water temperature to (35°C) and adding rapid 

stirring while soaking. 

2. Depth: Spray Simple Green into depth port openings and use pipe cleaners to remove 

any contaminant. 

3. ROX DO Membranes: The optical probe DO membrane would also benefit from a 

warmer soapy water temperature. Stirring or gentle sweeps with a soft paint brush across 

the membrane should aid in cleaning. 

4. Wipers: Replace all wiper pads on a contaminated unit. Cleaning of EDS or V2‐4 bristle 

type brushes may not be possible. If the bristles remain sticky after cleaning the brush 

must be replaced. 
171 

Instrument Deployment 

If you need to prepare YSI instruments to deploy into water contaminated with crude oil, 

YSI suggests the following procedure. Crude oil is can be thick and sticky, and we cannot 

guarantee the same performance intervals of our sensor membranes and wipers as under 

normal conditions. 

You will need: 

• YSIC‐Spray nanopolymer coating 

• Disposable plastic bags (Grocery store type) 

• Rubber bands 

• Light weight line or cord 

• Dawn dishwashing liquid 

• Buckets 

• Soft brushes for cleaning 

• Replacement brushes and wipers and hex wrench 

Procedure: 

1. Apply C

‐

‐Spray protective coating to exterior of instrument, sensors, and cable, according 

to the C Spray instruction sheet. 

• Recent testing has demonstrated that C Spray has no negative impacts on YSI optical 

sensors, ROX membranes or YSI pH probes. 

• ROX: Spray on and disperse over memb

‐

rane and probe face. Allow to sit 5 minutes and 

wipe off excess with a Kimwipe 

• YSI pH: Spray probe body including bulb and junction area. Allow to sit 5 minutes, and 

shake off excess. 

• All other optical sensors: Remove wiper, spray onto probe face and allow tosit for 5 

minutes. Remove excess with Kimwipe and polish probe face with dry Kimwipe to 

remove and streaking. Reinstall wipers. 

2. Calibrate the sonde after application like you normally would. 

3. For sampling applications, try one of the three following methods in order to deploy a 

sonde below a surface oil slick without impacting the sensors (see illustrations): 

Deployment Methods: 

1. Dispersants 

• If the oil film is light you can spray a dispersant onto the water surface before you 

lower the sonde. Mix “Dawn Dishwashing Soap” 50/50 with tap water in a squirt 

bottle. 
172 

2. Plastic Bag—This method works best with heavier 

instruments such as YSI 6600, 6920, 6820 sondes 

i. Place sonde in disposable plastic bag. 

ii. Cut off bottom of bag. 

iii. Gather bottom of bag around bottom of 

sonde/sensor and use a rubber band to close the 

bag. 

iv. Place second rubber band around the bag and 

body of sonde, below the bag handles. 

v. Attach a thin, sturdy line to bag handles. 

vi. Deploy sonde vertically and lower it through and 

below oil layer 

vii. Pull up on the line attached to the bag to pull up 

the bag and reveal the sensors to the water. You 

may need to “bounce” the line in order to push it 

through the opening. 

viii. When finished sampling, use an oar or other object 

to break apart the oil on the water surface before 

pulling instrument out of the water

ix. Rinse instrument in bucket of soapy water. Brush 

clean. 

x. Remove bag and dispose properly 

xi. If necessary, replace wipers and brushes on 

instrument 

xii. Repeat process with bag for next deployment 
173 

3. PC Tube

i. Tape one layer of plastic or foil to the 

bottom a PVC tube long enough to 

penetrate into water below the surface oil. 

ii. Place sonde or handheld sensor inside PVC 

tube. 

iii. Deploy sonde and tube vertically and lower 

it through and below oil layer. 

iv. Drop or push down on sonde or sensor 

while holding tube steady. The sonde will 

break through the foil, exposing the 

sensors to the water.

v. When finished sampling, pull instrument 

up through the tube. 

vi. Rinse instrument and tube in bucket of 

soapy water. Brush clean. 

vii. If necessary, replace wipers and brushes on 

instrument. 
174 

Disposing of Oil‐Contaminated Water or Materials 

If you generate waste liquids and/or waste materials while cleaning, consult your local waste 

disposal contractors and waste water treatment authorities, or local regulatory agencies, for 

requirements associated with proper handling and disposal of these materials. 

YSI Oil Decontamination & Deployment Procedures 5‐18‐2010 
175 

Attachment 2. IN SITU, Inc.: Cleaning and Care of Multiparameter Sondes and 

Sensors (Published with permission.) 

General Cleaning

Rinse the instrument body well, especially if it has been in contact with contaminated 

media. Level of cleaning for sensors/sonde/cable should be determined based on the 

level of contaminant exposure that has occurred.

For minor exposure follow general care instructions found in the following documents. 

Rinsing with warm soapy water and a soft bristle brush should remove moderate 

amounts of oily contaminants. Use commercial dish detergent for standard cleaning. 

Simple Green can also be used if more significant exposure occurs. If pH, DO and 

RDO sensors are removed, OxiClean can be used for sonde body and cable.

Air-dry or wipe with a lint-free tissue. Ultrasonic cleaning is not recommended. Follow 

all manufacturer recommended calibration procedures after cleaning has been 

performed. 

O-ring Replacement

O-rings should be replaced if the sensors have been exposed to oily contaminants and 

sensors have to be removed from the ports for cleaning. In all other situations, the orings should only be replaced for annual maintenance on the instrument (replace 

battery compartment o-rings as well).

If the o-rings become damaged to the extent that they no longer provide an effective seal, 

they should be replaced. If there is any doubt whether the o-rings should be replaced, it 

is best to err on the side of safety and replace them.

Before replacing o-rings, clean all mating surfaces, including the o-ring grooves.

O-rings and lubricant are included in the MP TROLL 9000 Maintenance kit available 

from In-Situ Inc. or your distributor.

Conductivity Sensor

Check the sensor for decline in sensitivity of the electrodes. If necessary, flush the sensor 

with water, or swish in a mild detergent solution and rinse with tap water. A swab or 

soft-bristle brush may be gently used to clean the electrodes. Remember that the 

electrodes are made of graphite, which is soft and easily damaged.
176 

pH, pH/ORP

If the platinum ORP sensor appears dull or oil-coated, it may be cleaned with a cotton 

swab dipped in alcohol. Rub gently until the platinum appears shiny. Rinse in clean 

water.

If a film develops on the glass electrode, or if the sensing glass or junction becomes 

dehydrated, the response may be sluggish or erratic, or the sensor may fail to calibrate. 

In these cases, rinse the sensor in 90% isopropyl alcohol and soak in a storage solution 

(Catalog No. 0065370) for at least an hour or overnight if needed. If this does not restore 

the response, try soaking in 0.1 M HCl solution for 5-10 minutes, followed by a thorough 

rinse in clean water. Replace junction and reference filling solution after cleaning.

Typical cleaning: First, rinse the sensor tip under a running cold water faucet or use 

a gentle jet of clean water from a rinse bottle. If this is not sufficient select the specific 

method (or combination of methods) from the list below. After any of these methods 

have been applied, prepare the sensor for subsequent use by rinsing the sensor tip 

with water followed by an overnight soak in pH 4 buffer. Replacing junction and 

reference filling solution should be done if contaminant exposure occurs.

Oily or greasy residue: Use warm water with mild soap. Follow with a generous 

water rinse. Isopropyl alcohol can be used for short soaking periods of up to an hour. 

Strong solvents (chlorinated solvents, ethers, or any ketones including acetone) must 

be avoided.

Protein-like material, or slimy films: First clean the sensor in mild soap and warm 

water. Then soak in a 0.1M HCl solution for 10 minutes and rinse with DI water.

RDO

Cleaning the Sensor

1. Leave the cap on the sensor!

2. Rinse the sensor with warm soapy water and a soft bristle brush.

3. Replace sensing cap as needed.

Note: If any damage to the black layer of the sensor has occurred due to contamination, 

the sensing cap should be replaced to ensure accurate readings.

Do not use organic solvents—they will damage the foil. Do not remove the cap from the sensor prior to brushing. After 

cleaning the sensor, perform a 2-point user calibration.

If extensive mineral build-up is present, soak the cap end in vinegar for 15 minutes, then 

soak in deionized water for 15 minutes.
177 

Cleaning the Optical Window (Perform only if changing the cap)

Remove the cap and gently wipe the window with the supplied lens wipe.

Caution: Do not wet the lens area with water or any solution.

Clark Cell DO

Inspect the sensor and membrane if readings begin to drift.

• Check for discoloration of the electrodes due to silver chloride (AgCl) deposition.

• Inspect the membrane for integrity of the surface, for the presence of algal growth or 

other contaminants, for crystallization that may indicate a leak in the membrane, and to 

ensure no air bubbles are trapped under the membrane.

Remove the membrane module and clean the electrodes as follows: 

Cathode. Use a polishing strip to buff the platinum cathode until it is shiny. This 

removes any deposits, increasing the chemically active surface of the electrode for a 

stronger D.O. signal. Anode. If the sensor appears to be excessively discolored from its 

original matte grey color, clean the anode with ammonia and a soft brush. Extreme 

discoloration may be removed by soaking for a half-hour in ammonia before cleaning 

with a brush.

The surface of the anode should appear uniform, but not necessarily mirror-like.

Regular cleaning will prevent pitting of the anode surface, caused by accumulated silver 

chloride deposition. Severe pitting cannot be removed; the sole remedy is to replace the 

sensor. 

After cleaning, rinse thoroughly and shake to dry. Then fill and attach a new membrane 

module as follows.

Replacing the Membrane Module

The D.O. sensor performs best in clean water. In environments with high organic 

content, the membrane performance can be affected ed. Rips, tears and other damage 

will also affect membrane performance. For best results, replace the membrane when 

the slope and offset calculated during calibration change dramatically.

The current applied is so small that the electrolyte solution can be expected to last 

longer than the membrane in most applications

To replace a membrane module:

1. Make sure the area around port 2 is free of dirt and moisture, then remove the sensor. 

Remove and discard the used membrane module.

2. Inspect and clean the sensor as needed (see above).
178 

3. Fill a new membrane cap with electrolyte and attach it to the sensor.

Refer to “Fill the Membrane Module” in the instrument manual.

4. Install and condition the sensor. Refer to “Condition a Newly Installed Sensor” in the 

instrument manual.

Remember to condition the sensor for at least 2 hours, preferably 10 hours, before recalibrating with a new membrane. 

Even with all visible air bubbles removed, a certain amount of gas will be trapped under the membrane. The conditioning 

period will remove this excess oxygen.

Turbidity

The optical windows of the sensor are made of scratch-resistant sapphire. The optical 

components are not user-serviceable. Serious mechanical and temperature shock are 

about the only things that can damage the LED. Follow general cleaning instructions for 

cleaning oily contaminants from the sonde. If you feel the instrument has suffered such 

damage, contact In-Situ Technical Support.