Sediment Sampling Guide and Methodologies (second edition)

Sediment Sampling Guide

and

Methodologies

State of Ohio

Environmental Protection Agency

Division of Surface Water

November

2001

P.O. Box 1049, Lazarus Government Center, Columbus, Ohio 43216-1049

Robert A. Taft, Governor

Christopher Jones, Director

(2nd Edition)

Ohio EPA Sediment Sampling Guide

Ohio Environmental Protection Agency

Lazarus Government Center

P.O. Box 1049

Columbus, Ohio 43216-1049

TABLE OF CONTENTS

DEFINITIONS ................................................................. 1

1.0 - SAMPLING PURPOSE ................................................... 3

a. Bioassays ............................................................ 3

b. Biosurvey Sampling .................................................... 3

c. Monitoring ............................................................ 3

d. Contaminant Source Identification ......................................... 3

e. In-Situ Measurements ................................................... 3

f. Dredging / Section 404-401 Decisions ...................................... 3

g. Trends / Historical Contamination ......................................... 4

h. Complaint Investigation ................................................. 4

I. Sediment Collection Technique Evaluation .................................. 4

j. Nonpoint Pollution Assessment ........................................... 4

k. Nutrient Cycling ........................................................ 4

l. Bedload / Sediment Dynamics ............................................ 4

2.0 - SAFETY .................................................................. 5

3.0 - SAMPLING PLAN ........................................................ 6

a. Description of the Project ................................................ 6

b. Data Quality Objectives ................................................. 6

c. Previous Studies ....................................................... 6

d. Dates of Collection ..................................................... 6

e. Sample Site Selection .................................................. 7

f. Estimating Particle Size Percentages ...................................... 7

g. Sample Types ......................................................... 7

h. Field Screening ........................................................ 8

i. Parameter Selection .................................................... 8

j. Site and Sample Description ............................................. 8

k. Sample Preparation and Handling ......................................... 9

l. Statistics .............................................................10

m. Station Replicate Samples .............................................. 10

n. Blanks / Field Duplicate Samples ......................................... 10

o. Reporting ........................................................... 10

Ohio EPA Sediment Sampling Guide

4.0 METHODOLOGIES ....................................................... 11

a. Bathymetric Survey / Initial Reconnaissance ................................ 11

b. Pre-sample Collection ................................................. 11

c. Changing Sampling Site Locations ....................................... 11

d. Decontamination / Cleaning / Calibration ................................... 12

e. Suggested List of Supplies / Equipment for Sediment Collection ................ 12

f. Preparation for Sampling / General Methodologies ........................... 12

g. Standard Surface Grab Collection with Scoops and Spoons ................... 13

h. Standard Surface Grab Collection with Dredges ............................. 13

i. Standard Core Collection ............................................... 14

j. Other Types of Collection ............................................... 14

k. Compositing ......................................................... 15

l. Sample Preservation .................................................. 15

m. Holding Times ........................................................ 15

n. Other Data Collection .................................................. 15

o. Sample Labeling/ Shipping/ Paperwork / COC .............................. 16

5.0 DATA REPORTING AND STORAGE ...................................... 17

a. Data Reporting ....................................................... 17

b. Data Storage and Retrieval ............................................. 17

APPENDICES

A. Collecting Sediment samples by Vibro-coring ............................... 18

B. Sediment Oxygen Demand ............................................. 21

C. Sample Collection for Solid Phase Sediment Bioassay ........................ 23

D. Standard Sampling Form ............................................... 26

E. Table of Sediment Sampling Equipment ................................... 27

F. Sediment Sample Volume and Container Type for Samples

Submitted to Ohio EPA DES Laboratory ................................... 30

G. Sediment Sampling Locations ........................................... 31

BIBLIOGRAPHY ............................................................. 35

DEFINITIONS AND ABBREVIATIONS

ACOE - United States Army Corps of Engineers

Aliquot - A portion or subset of a sample. An

aliquot can be any size, but it must be

representative of the parent sample.

Background - Refers to the concentration of a

chemical at an upstream site or other location

having similar physiochemical characteristics

which can be compared to the concentration of

the same chemical found at the site of interest.

BNA - Base Neutral Acid extractible compound

Cleaned - Equipment and supplies that have

been washed with water and detergent and rinsed

with local water or tap water followed by a rinse

with deionized water to ensure there is no

carryover of VOCs and metals from the tap water

to the equipment.

COC - Chain of Custody

Composite Sample - A thoroughly homogenized

set of two or more grab samples.

Contaminated Sediment - A sediment where the

concentration of a chemical exceeds a level of

toxicological concern.

Decontaminated - Equipment and supplies that

have been cleaned and subjected to

decontamination rinses using the procedures set

forth in section 4.0(d) of this manual.

DERR - Ohio EPA Division of Emergency and

Remedial Response

DES - Ohio EPA Division of Environmental

Services

DQO - Data Quality Objectives

DSW - Ohio EPA Division of Surface Water

Field Duplicate - An aliquot of a sample collected

to make an exact copy of the original sample.

Often referred to as a split sample. Duplicate

samples are used to check sample preparation

techniques, laboratory precision and comparison

of different laboratory results.

GLNPO - Great Lake National Program Office

Grab Sample - A single, discrete sample collected

from one location at one point in time.

Impacted Sediment - A contaminated sediment

where an adverse biological impact is observed.

Local Water - Stream or lake water collected near

the sediment sample.

Naturally Occurring Aquatic Substrate - Solid

materials associated with surface waters and not

of anthropogenic origin on or within which

organisms can live.

PAH - Polycyclic Aromatic Hydrocarbons

PCDD - Polychlorodibenzodioxins

PCDF - Polychlorodibenzofurans

Project Manager - For the purposes of this

document, a person that is responsible for the

design, implementation and reporting of a

sediment sampling project.

QA/QC - Quality Assurance/Quality Control

Reference Sediment - Refers to the concentration

of a chemical at an Ohio EPA ecoregional

reference site which represents conditions of least

impact as a result of known human activity.

Sediment - Unconsolidated inorganic and organic

material that is suspended in and being

transported by surface water or has settled out

and deposited under surface waters. Sediment

includes: 1) materials below the water surface

under bankfull conditions in streams, lakes, and

ditches; 2) materials at normal pool elevation for

reservoirs; 3) materials within the federal

jurisdictional boundaries of wetlands; 4) materials

at and below maximum capacity for ponds and

lagoons; 5) for Lake Erie, materials found at or

below high water conditions as defined by the

Ohio EPA Sediment Sampling Guide

United States Geological Survey over a five year

period.

SOP - Standard Operating Procedure

Station/ Field Replicate - Samples from a location

that were taken in the same general area (e.g., 20

to 200 meters depending on waterbody), during

the same time period, using the same sampling

equipment (decontaminated between samples),

and using the same sampling techniques as the

original sample. Station replicates are usually

used to determine sample variability at a given

location at a given point in time.

Synoptic Survey - A general investigation of a

large geographic area. Usually a basin wide

study.

TCLP - Toxicity Characteristic Leaching

Procedure

TPH - Total Petroleum Hydrocarbon

U.S. EPA SW-846 - A document containing test

methods for evaluating solid waste. SW-846

provides test procedures & guidance which are

recommended for use in conducting the

evaluations and measurements needed to comply

with the Resource Conservation and Recovery

Act (RCRA).

USGS - United States Geological Survey

VOC - Volatile Organic Compound

40 CFR Parts 87 to 149 - The Code of Federal

Regulations is a codification of the general and

permanent rules published in the Federal Register

by the Executive departments and agencies of the

Federal Government.

OHIO EPA SEDIMENT SAMPLING

GUIDE AND METHODOLOGIES

1 - SAMPLING PURPOSE

Sediment samples are collected by the Ohio EPA

for a variety of reasons including chemical,

physical, toxicological and biological analysis.

Due to the inherent variability of sediments,

collection techniques should be evaluated and

chosen for each sampling site and each sampling

purpose. Choosing the most appropriate

sampling device and technique depends on: 1)

The purpose of the sampling; 2) the location of

the sediment; and 3) the characteristics of the

sediment. This document should be used only as

a guide for selecting the sampling location and

proper collection technique (Appendix E contains

a table that can be used as an aid in selecting the

most appropriate sediment collection device).

Once the sampling site and collection technique

have been selected, then the specific

methodologies for the actual collection of the

samples should be closely followed. The

experience and judgement of the sample collector

should be used as much as possible in order to

obtain a representative sample of the sediment

environment compatible with the objectives of the

sampling. Whatever sampling technique and

device is used, the specific rationale and

collection methodologies should be stated in each

evaluation and report of the data. Users are

encouraged to review other references such as

Plumb (1981), Burton and Landrum (1990),

Mudroch and MacKnight (1994), and Mudroch

and Azcue (1995) for background information and

additional guidance.

The purpose of the sediment sampling should be

well defined before any sediment sampling plan

is developed. Below are brief descriptions of

sediment sampling projects that have been used

in environmental studies.

1a. Bioassays

Sediment bioassay samples are used to

determine if there is toxicity to representative

aquatic organisms from contaminated bulk

sediments. Sediment bioassay samples are

usually collected within the top 10 centimeters of

the sediment surface with equipment that causes

the least disturbance to the sediment surface

during collection. Specific methodologies have

Section 1

not been developed by Ohio EPA for collection

of pore waters or elutriate tests for bioassay.

1b. Biosurvey Sampling

Macroinvertebrates are often collected for

biosurveys from soft, fine grained sediments.

Biosurvey sampling is addressed in Part V,

Section A of the Manual of Ohio EPA Surveillance

Methods and Quality Assurance Practices,

Volume I (1991).

1c. Monitoring

Chemical and physical analysis of sediments can

be used as a tool for the monitoring of pollutant

discharges to a river or lake system. In order to

be able to make valid comparisons among

stations or reference sites, consistent sampling

techniques should be maintained. Samples

continue to be collected from the Ohio Stream

Regionalization Project sites and other

"reference" sites to improve the data base for

background conditions within each established

ecoregion. These data can then be applied as

reference for evaluation of contaminated areas.

1d. Contaminant Source Identification

Sediments can be used to help locate nonpoint,

historical, or intermittent discharges that may not

be readily apparent using samples collected from

the water column. Sediments are used to identify

the location of these sources by upstream

incremental collection of samples from a

contaminated site.

1e. In-situ Measurements

Sediment oxygen demand (SOD) is an in-situ

measure of the oxygen consumed by biochemical

decomposition of organic matter in stream or lake

sediment deposits. SOD can be used to evaluate

pollutant source control performance or as a

metric (input) for use in water quality models.

1f. Dredging / Section 404-401 Decisions

Sediment samples are often collected for use in

dredging and dredge spoil management

decisions. These samples should be collected

within the vertical profile of the dredging project to

Ohio EPA Sediment Sampling Guide

account for probable stratification. Discrete

sampling is preferred and the use of composite

samples for dredge management decisions

should be made with caution. In known or

suspected heavily contaminated areas, special

analyses such as PCB tests and RCRA regulated

compounds using the Toxicity Characteristic

Leaching Procedure (TCLP) in U.S. EPA SW-846

should be performed to aid in disposal decisions.

In addition, whole sediment toxicity tests have

been developed to aid in disposal decisions and

complement the TCLP test.

1g. Trends / Historical Contamination

Sediment sampling is also used as a tool in the

evaluation of the effectiveness of pollution source

controls. This can be accomplished with discrete

vertical sampling (assuming the sediments have

not been mixed or otherwise disturbed) or by

reproducing earlier sampling efforts.

1h. Complaint Investigation

Sediment sampling to help address citizen

complaints requires a great deal of assessment

and judgement by the sample collector. The

design of each complaint sampling investigation

should be evaluated on a case by case basis.

Because of cost and often long turn around times,

sediment sampling for the sole purpose of

resolving citizen complaints should be used

judiciously.

1i. Sediment Collection Technique Evaluation

Comparison of samples using sediment collection

techniques and devices can be made to

determine the easiest and most effective

sampling method. Evaluation of other techniques

such as sediment traps can also be made to

make sediment collection more reproducible.

1j. Nonpoint Pollution Assessment

Sediment samples can be collected for evaluation

of nonpoint pollution. Selection of parameter

coverage for analysis of the samples can

sometimes be important in defining the source of

sediments (e.g., high pesticide/herbicide

contamination would indicate agricultural run-off).

1k. Nutrient Cycling

Sediment samples can be collected in lake or

river habitats to determine potential release of

nutrients (e.g., phosphorus) back into the water

column.

1l. Bedload / Sediment Dynamics

Prediction of sediment resuspension, both

modeling and measurement procedures, are still

experimental. The dynamics of the movement,

transport and fate of contaminants adsorbed to

sediment is not thoroughly understood and are

beyond the scope of this document.

OHIO EPA SEDIMENT SAMPLING

GUIDE AND METHODOLOGIES

2 - SAFETY

Prior to the development of the sampling plan,

Ohio EPA safety policies should be consulted.

Everyone involved in the preparation, collection

and analysis of the sediment samples should be

familiar with the safety policies. Special attention

should be given to physical dangers such as slip,

trip and fall hazards when working around water.

In general, it is recommended that the sample

collector(s) avoid skin contact with all sediments

and inhalation of odor should be avoided. Special

precautions may have to be taken when working

with contaminated sediments especially near

potential or known contaminant sources such as

unpermitted outfalls, NPDES permitted outfalls,

landfills or hazardous waste sites. Specific site

safety plans for sampling near unregulated

hazardous waste (DERR) sites should be

followed when sampling is done in conjunction

with a DERR project or any other project where

contaminated sediments may pose a risk to

sampling personnel.

Section 2

OHIO EPA SEDIMENT SAMPLING

GUIDE AND METHODOLOGIES

3 - SAMPLING PLAN

Sediment sampling usually entails relatively

higher expense in personnel, collection effort and

analytical costs per sample than the collection

and analysis of water samples. A sampling plan

should be developed, written and approved by the

project manager prior to the collection of sediment

samples to maximize resource allocation. The

plan should incorporate a statement as to the

purpose and the data quality objectives of the

proposed sediment sampling.

Sample collection is often governed by logistic

and resource constraints rather than specific

project objectives. As a result, the data from such

studies are often incomplete and the benefits

from the collection of that data is reduced if not

eliminated as a result of the constraints. If

resources are unavailable to perform an adequate

study to meet the data quality objectives, then the

sampling project should be reevaluated.

3a. Description of the Project

A brief description of the sampling project should

be included in the sampling plan. A description of

how the sediment sampling will be integrated with

other planned studies and an explanation of how

the sediment sampling information will be used

should be stated.

3b. Data Quality Objectives

This important section of the sampling plan

should state what type of information needs to be

collected in order to meet the objectives of the

sampling project. This information should

include:

C Purpose of the sampling.

C How the data from the sampling will be used.

C What actions will be taken as a result of the

sampling.

C Identification of the laboratory performing the

analyses.

C The parameters for analysis including method

detection limits (see Part VI of the Manual of

Ohio EPA Surveillance Methods and Quality

Assurance Practices if the Ohio EPA laboratory

is being used).

Section 3

C Number and type of quality control samples

such as field blanks, equipment rinses, field

duplicates, station replicates, reference and

background samples.

C Statistical analysis and criteria (allowable

errors) used to evaluate the data.

C Standards, background or benchmark criteria

used to compare the analytical results.

C Number and location of samples to be collected

to meet the purpose of the project.

C How the information will be reported.

C Whether the data will be entered into an

electronic database and, if so, the structure and

file type of the database.

3c. Previous Studies

A thorough review and assessment of existing

data and information of the sampling area should

be performed to assist in this portion of the

planning process. A brief summary of that

information and an assessment should be

included in the written sampling plan. In

reviewing existing information, attention should be

given to the purpose of the collection of the

historical data and what sampling techniques,

analytical procedures and laboratories were used

in performing the analyses. This information is

important in order to determine the usefulness of

the historical data for the proposed project.

3d. Dates of Collection

The general time of year when the samples will

be collected should be considered during the

planning of the sampling activities. In general,

sediment sampling in the low flow conditions of

summer and fall are the most practical. Seasonal

variations of sediment deposits and quality can

occur due to high flows and ice scour on rivers,

leaf litter in the fall, land use practices (e.g.,

agricultural pesticide applications) or seasonal

variations in benthic populations. Winter may be

a convenient time to sample some inland lakes

through the ice, while ice cover may be a severe

safety concern in the collection of river sediment

samples. The analytical laboratory should be

contacted early in the planning process for proper

coordination to ensure all needs are met.

Ohio EPA Sediment Sampling Guide

3e. Sample Site Selection

Selection of the sampling locations and number of

samples is one of the most important decisions to

be made in the planning process. The selections

should be made based upon the data quality

objectives of the study and resources available to

the project. Rationale for the selection of the

sampling locations should be included in the plan.

The chemical and physical nature of sediments is

strongly influenced by the size of the individual

particles of sediment. Sediments composed of

sands (0.06-2.0 mm) and larger sized particles

are often stable inorganic silicate minerals.

These larger particles form non-consolidated

deposits, have a relatively lower specific capacity

(amount of interstitial water) and a more neutral

surface electrical charge. These types of

materials are usually not associated with

contaminants and are not recommended for

analysis. Fine grained silts and clays (<0.06 mm),

however, have a much larger specific capacity,

have unbalanced electrical charges and much

larger surface area to volume ratio. These

properties make the finer grained sediments

much more chemically, physically and biologically

interactive. These are the types of sediments that

should be submitted for analysis and most of the

sediment sampling locations should be biased

towards collecting these types of sediments (see

Appendix G).

3f. Estimating Particle Size Percentages

A goal of sediment collection is > 30% silt and

clays in the sediment sample. If these sediment

types are not found, then it should be noted on

the laboratory submission sheets and field

collection form. The percentage of silts and clays

in a sample can be estimated in the field by

marking a line on a clear jar and then marking

30% of the way up to that line on the jar with

another line. Fill the jar to the top line with

sediment and vigorously shake the jar and set

aside to settle. A one inch headspace in the jar

allows for easier mixing. After settling for 10

minutes, an estimate of the particle size

distribution can be made with a visual inspection

of the sediment stratification in the jar. If the fines

stop below the 30% line, then the silt/clay fraction

is likely to be <30%.

It's assumed that the finer grained sediments are

located in still waters of the sample area in deep

water, at stream margins, behind boulders and

other obstructions, or at inside bends of river

meanders. An initial reconnaissance of the

sample area should be performed, if possible,

prior to the completion of the sampling plan. This

reconnaissance can often identify field limitations

in the study design that can be addressed prior to

sample collection. An initial reconnaissance

should include a cursory bathymetric survey using

a wading staff in shallow streams and rivers or an

echosounding (sonar) depth finder for deeper

waters. Local knowledge or recent navigation

charts (USGS surveys or ACOE harbor/waterway

soundings in navigable waters) can often provide

similar information to an echosounding survey.

3g. Sample Types

A description and rationale for the types of

samples to be collected should be included in the

written plan.

Cores - Vertical discrete grab samples. Most

appropriate for historical contamination

information or dredging decisions at heavily

contaminated areas.

Cores - Depth integrated composite samples.

Most appropriate for reference and Section

404/401 issues.

Scoops and Dredges - Surface (top two to four

centimeters) sediment grab samples. Most

appropriate for benthic, sediment oxygen

demand (in-situ), recent ambient conditions and

recent contaminant investigation.

Scoops and Dredges - Surface sediment

composite samples. May be used to reduce

costs for specific conditions/situations such as

some Section 404/401 issues or ambient or

specific historical data. In general, however,

discrete sampling is preferred if resources are

available. An example of a discrete sample

would be taking a section of one centimeter of

sediment from a core sample that was originally

one meter long.

Ohio EPA Sediment Sampling Guide

3h. Field Screening

The use of field screening devices such as head

space analysis with Photo Ionization Detectors

(PID) and Flame Ionization Detectors (FID) is

encouraged for intensive sampling programs. A

preliminary screening program or “phased

approach” can give a lot of direction as to where

more intensive sampling is needed and can give

insight as to the types of analyses which may or

may not be needed for subsequent sampling

phases. These field screening devices have

different sensitivities to different compounds. In

general, PIDs are more useful for detection of

chlorinated and aromatic compounds while FIDs

are more useful for aliphatic compounds.

To use this technique, an aliquot of sample is

placed in a glass jar and covered with aluminum

foil. After the atmosphere in the jar has reached

equilibrium with the sediment, the PID or FID

probe tip is inserted into the jar through the

aluminum foil and the measurements recorded.

Action level criteria for head space analysis

results should be specified in the data quality

objectives section of the sampling plan. Head

space analysis tests must be performed only by

personnel specifically trained in the use of these

instruments.

3i. Parameter Selection

Selection of the chemical and physical analysis to

be performed on each sample is based upon the

purpose of the study, the data quality objectives

and available resources. Each sediment sample

should be analyzed, at a minimum, for Total

Organic Carbon (TOC) and Particle size. All

analyses should conform to SW-846, 40 CFR Part

136, Manual of Ohio EPA Surveillance Methods

and Quality Assurance Practices, or Standard

Methods as appropriate.

Possible analyses include:

CHEMICAL

C Total Organic Carbon (TOC)

C Metals (Pb, Ni, Cu, Zn, Cd, Cr, Fe, Mn, Hg, As

and other metals as necessary)

C Nutrients (COD, Total Phosphorus, Total

Kjeldahl Nitrogen (TKN), Ammonia)

C Cyanide

C Oil and Grease

C Persistent Organics (Pesticides, Insecticides,

Herbicides, PCB's, BNA's, TPH's, PCDD,

PAH's, and PCDF's in special circumstances)

C Volatile Organics (including trihalomethanes)

C Volatile Sulfides

C Oxidation Reduction Potential(ORP)/redox

C pH

PHYSICAL

C Particle size

C Appearance/Texture/Odor/Color

C Radiochemistry

C Shear strength and water content (for dredging

purposes only)

BIOLOGICAL/BIOCHEMICAL

C Sediment Oxygen Demand (SOD)

C Bioassay

C Macroinvertebrate Survey

OTHER DATA COLLECTION

C Overlying water quality including: Water

Temperature, Water Depth, Dissolved

Oxygen, Conductivity, pH, Turbidity, Water

Velocity.

3j. Site and Sample Description

Each sample station should have the following

information recorded:

C Date and time of the sample collection.

C Latitude/Longitude of site.

C River Mile of site from PEMSO maps, if

available.

C Location description with reference to visual

landmarks.

C Sampling location marked on a 7.5 minute

USGS Quadrangle map (to show exact location

of grab sample). More detailed custom maps

should be made as needed.

C Water Depth/Results of bathymetric survey.

C Description of current.

C Unusual conditions (weather, equipment

malfunction, ship traffic, etc.).

C Photographs of samples (close up) and sample

locations are recommended.

C Physical description of sample (color as

determined by the Munsell

soil color chart,

texture, odor, obvious materials such as coal

fines, metallic chips, oil and grease, etc.

Ohio EPA Sediment Sampling Guide

C Collection device used.

C Grab or composite sample (include detailed

compositing information if not a grab).

C Indicate collection of field duplicate or replicate.

C Sediment depth used for sample (i.e., 1-3 cm;

10-15 cm etc.).

C Sampling crew members.

C Field measurements performed such as head

space analyses and water temperature, pH,

conductivity, dissolved oxygen and turbidity.

C Any site codes used to I.D. the sample station.

C The sediment collection form included in these

methodologies (Appendix D) can be used to

record the site and sample description

information.

3k. Sample Preparation and Handling

This section of the sampling plan should detail the

appropriate sample collection and handling

procedures.

Compositing - A brief description of type of

composite and compositing techniques.

Sample Volume and Container Type - The

volume of sample and type of container should

be listed in the plan for each sample collected.

The sample container type(s) must be

consistent with the container type(s) specified in

the methodology. Sample size should conform

to the request of the analytical laboratory

receiving the sample. Sediment samples

submitted to Ohio EPA’s DES Laboratory for

analysis should be collected into containers in

accordance with Appendix F. Volatile organic

samples should be collected as discrete grab

samples and packed to exclude as much air

space as possible. Surficial water from the

sediment sample may be added to exclude all

air. Because of field conditions, some samples

may not yield enough material for analysis.

These samples are to be handled on a case by

case basis. When this or other special

conditions occurs, contact the laboratory

sample coordinator for advice. Proper

communication between the sample collector

and laboratory is essential to ensure all needs

can be met.

Special Considerations - In special

circumstances to meet specific data quality

objectives, sediment samples may be sieved in

the field to a uniform screen or particle size.

The samples should be screened to retain

0.060 mm or smaller particles. In order to

calculate concentrations, the sediment volume

screened and the specific gravity of the

unscreened sediment must be known.

Sediment samples for VOC analysis should not

be screened. In addition, stream debris such as

rocks, sticks and leaves should be removed

from sediment samples.

Sample Labeling - All sample containers should

be labeled with the site name as it appears on

the laboratory submission form, the date and

time of the sample collection and the name of

the sample collector or other information

specified by the laboratory.

Preservation - All sediment samples for

chemical or bioassay analysis should be

immediately chilled and stored at 4EC.

Equipment Decontamination - A description of

equipment, supplies and decontamination

procedures should be included. For efficiency

and to reduce field decontamination activities,

all sampling equipment should be cleaned and

decontaminated at the laboratory or field office

before going to a sample site. It is easier to

clean and decontaminate as soon as possible

after returning from the field. If possible, a

separate set of cleaned and decontaminated

equipment should be available for each

sampling site.

Sample Handling and Shipment - Sample

containers should be placed in clear plastic

bags to minimize soiling of the shipping

container and to protect laboratory personnel.

Glass containers should be protected from

breakage. All sediment samples should be

chilled and stored in coolers or similar

containers at 4EC. A description of how the

samples were packed in the field, what

preservatives were used and how they were

shipped to the laboratory should be recorded.

A chain of custody form must accompany each

sample shipment.

Ohio EPA Sediment Sampling Guide

3l. Statistics

Refer to Sediment Sampling Quality Assurance

User's Guide (U.S.EPA 1985) for a more

exhaustive discussion of statistical analysis of

environmental sampling.

C Determine number of samples.

C Determine components of variance and

difference of means that are significant.

C Evaluate field duplicates/station replicates and

criteria for acceptance of data.

3m. Station Replicate Samples

Station replicate samples are a complete

separate collection of a sample at one site.

Station replicate samples can be collected to

determine the variability of the concentrations of

contaminants in the sediment at a specific site

and/or as an assessment of field sampling

techniques.

3n. Blanks / Field Duplicate Samples

The number and type of quality control samples

should be included in the sampling plan. Ten

percent (10%) of the sediment samples should be

collected as duplicates and 5% as blanks or

equipment rinses. Field duplicate samples are

collected to determine laboratory analytical

variability and/or field compositing techniques and

of sediment heterogeneity within a single

collected sample. Duplicates are collected by

“splitting” a sample that has already been

collected into two identical samples for analysis.

Equipment rinse samples for sediment samples

are comprised of a distilled and deionized water

rinse following equipment decontamination. Field

blanks are samples of uncontaminated silica sand

collected using the same sampling equipment

and techniques as the sediment sample

collections. The equipment rinse samples and

field blank samples are used to demonstrate that

significant amounts of contaminants are not

introduced into the sediment samples from

sampling equipment or sample handling.

3o. Reporting

A description of the format of the final report

should be included in the sampling plan. At a

minimum, the following data should be tabulated,

including:

C Calculation of mean, median, range and

number of samples for large scale synoptic

surveys.

C QA/QC sample results.

C Any deviations from the sampling plan.

Finally, the plan should be reviewed and the

question answered: Will the implemented plan

meet the stated sampling and data quality

objectives?

OHIO EPA SEDIMENT SAMPLING

GUIDE AND METHODOLOGIES

4 - METHODOLOGIES

Once the sampling plan has been completed and

approved, then the following methodologies

should be used for the actual collection of the

samples. Examples of sampling locations and

sediment types are identified in Appendix G.

4a. Bathymetric Survey / Initial

Reconnaissance

The starting point of the survey should be at a

location that is readily identifiable in the field and

that can be found and used at a later date to

reproduce the sampling.

Echo sounding surveys for lakes and large rivers

should be made from boats by moving slowly

along parallel lines perpendicular to the river

current and noting the reading on the depth

finder. The proposed sampling area should be

equally divided into 10 transects with depth

readings taken continuously or at least every 10

feet along the transects.

Operation of the depth finder should be in

accordance with the manufacturers instructions

and resolution of the sounder should be set for

the expected depth of the water. Sensitivity of the

depth finder can be set to determine relative

densities of the bottom.

The data from the survey should be recorded in

field notes and the deepest area used for sample

site selection.

In medium sized rivers, the river can be waded or

a boat used to determine the deepest sites using

a calibrated staff.

If bathymetric information is not available,

samples from free flowing rivers or streams

should be collected from:

C Both banks of a relatively straight section of a

stream or;

C On the inside edges of a meander or;

C In slack water or eddy current areas.

C In navigation channels and the Ohio River and

depending on the data quality objectives

(DQOs), samples should be collected far from

Section 4

the center of the dredged portion of the

channel/river on alternating sides of the

channel/river.

C On medium sized and smaller rivers and

streams, the use of hands, feet, fingers and

toes with the "Wading Braille" technique

(locating sediments by touch and feel) in

conjunction with best professional judgement

can be extremely effective in locating fine

grained deposits. This sampling technique is

the most commonly used technique by Ohio

EPA for sediment sample collection.

C Contaminant source investigations in lakes

should be biased towards the down current

(usually the eastern side for Lake Erie's Ohio

shore) side of littoral drift.

C Any contaminant source investigation should be

biased towards sampling sediments in the most

likely sink.

4b. Pre-Sample Collection

Collection of exploratory grab samples should be

used to revise sampling location in the field due to

unforeseen site conditions such as lack of

suitable sediment for sampling.

The person collecting the samples should be

open to revisions and able to adapt the sampling

design to meet unforeseen site conditions while

still meeting the data quality objectives of the

study. The sample should contain, as a goal,

more than 30% silt (<0.06 mm) or smaller particle

size by volume for an acceptable sample.

Use the soil classification description on the

sediment sampling form (Appendix D) to

determine the sample composition.

4c. Changing Sampling Site Locations

If exploratory grab samples do not meet the

criteria for the objectives of the study or the site

contains more than 70 percent sand or larger

particles, the location should be abandoned and

another location chosen.

If no other suitable location meets the criteria,

then a sample may be collected, but the results of

the analysis should be annotated in the report

Ohio EPA Sediment Sampling Guide

with a description of the sample.

The results of field screening techniques can be

used to determine appropriate sampling locations.

4d. Decontamination / Cleaning / Calibration

All collection equipment and supplies such as

dredges, corers, spoons, scoops and compositing

trays that may come into contact with the sample

should be cleaned prior to use as follows:

1 - Wash with Phosphate-Free Liquinox Soap

2 - Tap water rinse

3 - ASTM water (distilled water) rinse

4 - Methanol rinse

5 - Hexane rinse

6 - Allow to air dry

7 - Cleaned, decontaminated, and dried

equipment should be wrapped in aluminum

foil or sealed in reclosable plastic bags.

If field decontamination is necessary all Methanol

and Hexane rinses are collected in appropriate

containers for proper disposal at a later time.

All instruments must be calibrated before any

samples are collected. All portable units must be

calibrated with one or more calibration standards.

A log book/record must be properly maintained to

indicate which instrument or meter is calibrated,

date of calibration, standard concentration, age of

standards and field personnel. Good quality

control requires a known standard be used to

check the calibration before the sampling event.

All field instruments should have a written

standard operating procedure for each piece of

equipment which insures consistent calibration

requirements and proper maintenance.

4e. Suggested List of Supplies / Equipment for

Sediment Collection

C Sampler (Dredge, Corer, Scoop, SOD

Chamber, etc.)/extra weights/extra corer inserts

C Extra sample containers for sediment and water

samples. Be prepared for unexpected

additional sampling

C Depth Finder/ Calibrated Wading Staff

C Calibrated D.O./Temperature/Conductivity/pH

Meters/Turbidity

C Extra Rope

C Distilled and Deionized Water Wash Bottle(s)

C Distilled and Deionized Water for Field Blanks

C Teflon Solvent Wash Bottle

C Waste Solvent/Acid Collection Container

C Towels/Cleanup Supplies

C Plastic Trash Bags

C Ice and Sample Cooler(s)

C Sample Containers, Labels and Markers

C Leather, Latex, Neoprene or Rubber Gloves

C Rain Gear or Plastic Aprons

C Appropriate Safety Supplies

C Compositing Container/ Bowl and Mixing Spoon

C Rinse Bucket(s) and/or Water Pump and Hose

C Self Sealing Plastic Bags

C Clear tape for sealing container labels

C Shoulder Length Neoprene Gloves

C Chest Waders

C Field Notebook, camera

C PID/FID

C Duct Tape/Electrical Tape

C Sediment Collection forms

C Chain of Custody Forms

C GPS unit

C Munsell color chart

C Flow meter

C Topo maps with sample locations marked

C Copy of the sampling/ work plan

4f. Preparation for Sampling/General

Methodologies

While wading in shallow water, the sediment

collector should be standing on the downstream

side of the collection site. Care should be taken

to create the least disturbance to the sampling

site as possible especially from wading or

disturbance of the sediment from currents

induced by wading.

When using a boat or other sampling platform, all

engines should be turned off. The samples

should be collected upstream from the engines or

any other machinery that may release exhaust

fumes/oils into the sample.

Sampling equipment and supplies that may come

into contact with the sample should be cleaned

and decontaminated in accordance with the

decontamination procedures in the sampling plan.

In synoptic surveys, the most upstream or

reference sediment site should be collected first

to reduce chances of contamination between

Ohio EPA Sediment Sampling Guide

sites. If the sediment sampling locations are

located within a short distance of each other, then

the most downstream sample should be collected

first to avoid contamination from disturbance and

resuspension of sediment due to sampling

activities.

In general the finest grained sediments at each

sampling location should be collected and the

sample should contain, as a goal, more than 30%

coarse silt (<0.06 mm) or smaller particle size by

volume for an acceptable sample. Results of

headspace analysis can also be used to help

locate sampling sites.

Sampling in areas of aquatic vegetation where

macrophyte roots or other vegetation may be

collected should be avoided.

As much water as possible should be decanted

from the sample prior to placement into the

collection pan or bowl. Care should be taken

however to avoid loss of extremely fine material

from the sample during decanting.

A physical description and photograph, if

possible, of the undisturbed sample should be

made. The sediment collection form in Appendix

D should be used to record the sample

information.

For composite samples, the number of grab

samples collected for the composite should be

noted. The subsamples (grabs), of equal

volumes, should be placed in a cleaned stainless

steel or plastic basin. When all grab samples

have been collected, the sample should be

thoroughly mixed with an appropriate scoop or

spoon. Once mixed, a physical description and

photograph of the sample should be made. The

sediment should then be placed into appropriate

containers. Continuous mixing of the sample

should occur to prevent stratification of the

sample. The sediment collection form in

Appendix D should be used to record the sample

information.

All stones, shells, detritus, roots and other foreign

matter should be removed from the sample.

Samples for analysis of VOCs should not be

composited or homogenized and should be

collected first as discrete grabs. Containers

should be filled according to the following

sequence: Grab samples for VOC analysis first,

followed by composite samples for BNA's,

Pesticides/PCB's, nutrients, metals and particle

size.

4g. Standard Surface Grab Collection With

Scoops and Spoons

Scoops and spoons are inexpensive, widely

available, non-mechanical, very portable, able to

sample nearly every sediment type and easy to

use.

Scoops are used to collect sediment samples

primarily from shallow waters. Attaching the

scoop to telescoping poles allows for collection of

sediments in deeper waters.

Care should be taken when the scoop is raised

through the water column or is passed through a

river current during retrieval to minimize the loss

of extremely fine material.

With very little experience, a sampler can “feel”

the substrate with the scoop attached to a pole

and quickly find appropriate material for sample

collection.

Some disadvantages to using a scoop or spoon

includes: limited sample volume; possible loss of

very fine material during retrieval; not useable in

waters greater than 4-5 feet deep.

4h. Standard Surface Grab Collection With

Dredges

Surface sediment samplers (dredges) are

relatively inexpensive, are widely used and

available, are standard for some sampling

purposes (benthos), often don't need expensive

equipment to operate and come in a wide variety

of sizes.

The sampler should be “set” according to the

manufacturers instructions and lowered through

the water column. Dredges should never be

allowed to free fall into the substrate. The

sampler should be carefully lowered the last few

feet to minimize dispersal of fine material due to

a sampler induced shock wave.

Ohio EPA Sediment Sampling Guide

In shallow waters, some samplers can be pushed

directly into the sediment. Five and ten foot

extension handles can be attached to Eckman

dredges for sampling in shallow waters to plunge

the sampler into the sediment. These handles

can minimize some of the limitations of the

dredge.

The sampler is then tripped.

The sampler should be slowly raised through the

water column and placed in an appropriate

container (see the compositing section below). If

an insufficient or improper sample is collected,

additional weights should be added (if

appropriate) to the sampler to allow deeper

penetration into the sediment.

If additional weights do not help in the collection

of a sample, then the sampling equipment and

techniques should be reevaluated for the type of

sediment encountered.

For compositing, a minimum of three to five grab

samples (as near the same volume as possible)

from a site should be taken and thoroughly mixed.

An aliquot of that composite should be collected

and submitted as the sample for the site.

Some disadvantages to the use of surface

sediment samplers (dredges) include: shallow

depth of penetration; possible shock wave and

loss of very fine grained surface deposits;

potential for water column contamination and

nearby downcurrent sediment redeposition; loss

of depth profile; not appropriate for waters with

current (sampler drifts in current, “lies down” and

can’t be triggered); larger materials such as twigs

and stones prevents jaw closure; probable loss of

some water soluble and volatile organic

compounds; and it is possible to dilute the toxic

pore water with relatively clean surface water

(which is important in conducting sediment

bioassays).

4i. Standard Core Collection

Sediment corers are usually simple inexpensive

sampling devices, are manufactured in a variety

of materials, can collect samples at depth, can

maintain a more representative vertical profile of

the sediment stratigraphy, create less disturbance

by shock waves and can collect more highly

consolidated deposits.

Sediment corers are slowly lowered to the

substrate (gravity corers are released at the water

surface and allowed to free fall) and simply

allowed to penetrate the sediment under the

samplers own weight or pushed or vibrated

(vibro-core) into the sediments. Corers can be as

simple as homemade tubes of steel, plastic or

glass.

Commercial corers often contain core catcher

inserts (also known as chinese fingers or

eggshells) and one-way valves that allow the

sample to enter the tube, but not exit and to hold

it in place. Inserts should not be reused between

sample locations unless decontaminated.

Inserts made of plastic should not be used when

collecting samples for organic analysis. Upon

retrieval, the corer can be disassembled (e.g.,

split spoons, some core tips unscrew) and the

sample laid in a container or a prepared

decontaminated surface for further processing.

Cores from simple tubes and most other corers

often drop out or can be pushed out with a clean

rod.

Plastic or thin walled metal corers (or core liners)

can be cut, the ends capped, secured with tape

and the entire segment sent to the lab. This

process and the split spoon sampler reduces

contamination from one segment to another in

vertically stratified samples.

Detailed description of a vibro-core collection is

included in Appendix A.

Some disadvantages to the use of sediment

corers include: they do not work well with sandy

sediments; they collect limited sample volume

and very small surface area; they sometimes

require expensive and bulky equipment to work in

deeper waters and sediments.

4j. Other Types of Collection

In some cases, sediment can be collected directly

from the substrate by a diver using SCUBA gear

or supplied air.

C The sediment can be collected directly into the

Ohio EPA Sediment Sampling Guide

sample container or placed into the container

by the diver with a scoop and sealed and

composited at the surface.

C The diver should be downstream of the sample

site and should use caution not to disturb the

fine grained sediment at the substrate surface.

Coffer dams can be used in very small streams.

Coffer dams are temporary barriers that allow a

small segment of stream to be isolated from the

main water body and the isolated stream segment

de-watered. After de-watering, the sediment

inside the coffer dam can be collected with a

scoop similar to a soil sample.

C The coffer dam can be made by placing a 6"

diameter or larger pipe on the stream bottom

parallel to the stream current. This reduces

eddy currents and possible scour of the

sediment when installing the pipe as a coffer

dam.

C Quickly tilt the pipe vertically so the top of the

pipe is above the water surface.

C Care should be taken to avoid washing fines

from the sediment surface during installation of

the pipe.

C Once in place, the pipe should be pushed into

the substrate with a circular back and forth

motion.

C Water inside the pipe is removed by a pump or

by bailing.

C The sediment inside the pipe can then be

sampled with a simple scoop.

C Sieve samples for special circumstances.

Measure the volume sieved and the specific

gravity of unsieved sample to calculate

concentrations.

4k. Compositing

Preferred composition of the compositing

container:

C a plastic container for metals analyses

C a glass container for all types of analyses

C a stainless steel container for organics analyses

C a solid Teflon container for all types of analyses

(high costs usually prohibit its use)

Disposable aluminum trays are acceptable

compositing containers provided blank samples

or equipment rinses are collected from it prior to

use.

After a description of the sample is made, the

sediment is thoroughly homogenized with a

spatula or similar device comprised of a material

appropriate for the analysis performed. A

thoroughly homogenized sample is uniform in

color, consistency and water content. Care

should be taken to avoid spilling fines and

interstitial water during mixing.

Sampling equipment and supplies do not have to

be cleaned between subsamples of a composite

sample at a site. Equipment and supplies must

be decontaminated and cleaned between station

replicate sample collection and collections at

different sites.

All composite samples should be identified as to

the method of sample collection, depth and

volume of each discrete sample and the number

of samples per composite.

4l. Sample Preservation

All sediment samples for chemical, physical and

bioassay analysis should be cooled to 4EC as

soon as possible after collection.

4m. Holding Times

Samples for organic analysis should be extracted

within 14 days. Samples for metals, except for

mercury, must be analyzed within six months.

Sediment samples for mercury and nutrients must

be analyzed within 28 days.

4n. Other Data Collection

Field measurements for temperature,

conductivity, pH and dissolved oxygen should be

collected from the water column within one meter

of the sediment prior to sediment sample

collection. Depth profiles (at least surface,

mid-depth, bottom) for these parameters should

be made in waters that are too deep to wade.

The sampling location (with sufficient detail to

allow a revisit to the same sample location)

including latitude and longitude, river mile (if

available), a brief description of the sampling site

and information about unusual conditions should

be recorded for each location. A hand drawn map

of the sampling site showing landmarks and

depicting the sample location (including

Ohio EPA Sediment Sampling Guide

measurements from trees, etc.) can be very

effective in re-locating the exact sampling spot.

4o. Sample Labeling / Shipping / Paperwork /

COC

For samples submitted to the Ohio EPA

laboratory, procedures are the same as described

in Part III of the Manual of Ohio EPA Surveillance

Methods and Quality Assurance Practices Volume

I (1991). This manual should be used as guiding

principles for the information needed. Specific

procedures or forms should adhere to any

Administrative Order, contract or sampling plan

directive for samples submitted to non-Ohio EPA

laboratories.

OHIO EPA SEDIMENT SAMPLING

GUIDE AND METHODOLOGIES

5 - DATA REPORTING AND STORAGE

5a. Data Reporting

The data should be reported by the lab on a dry

weight (ug/g or mg/kg) basis.

Information to be included in any report of the

data include: rationale for site, sampling

equipment and analysis selection; a description of

how the sample location was found and recorded;

a map (preferably a 7.5 minute USGS Quad) of

the study area showing the sampling locations

(Latitude/Longitude and PEMSO River Mile);

sampling dates and type of sampling equipment

and methodologies used; sample handling and

preservation; sample COC; summary of QA/QC

samples; applicable statistics as identified in the

sampling plan. Analytical data reporting sheets

should include the sampler's name, station,

sample location, sample type, county, sample

number, collection date and time, date the sample

was received in the laboratory, date analyzed,

analytical methodology, data qualifiers, Method

Detection Limit (MDL) and Practical Quantitation

Limit (PQL). In addition to a list of parameters for

analysis, any comments need to be documented.

5b. Data Storage and Retrieval

Analytical data is to be entered into an electronic

database and include River Code, River Mile,

Location Description, Ohio EPA District, Latitude,

Longitude, STORET number, Waterbody ID

number, Ecoregion, if the location is a Reference

Site and collection information such as sampler

type, composite or grab, and depth of sample.

Section 5

Ohio EPA Sediment Sampling Guide

APPENDIX A COLLECTING SEDIMENT BY VIBRO-CORING

APPENDIX A - Collecting Sediment Samples

by Vibro-coring (Pole or Submersible)

Either of two types of vibro-coring systems:

A Rossfelder designed, submersible vibro-coring

system as used on the R/V Mudpuppy (see

EPA/GLNPO SOP); or

A Pole vibro-coring system per AScI design,

consisting of: electric vibrator motor (12 V DC)

and mounting plate with socket for attachment of

2” diameter extension poles; two, 12 V DC

storage batteries with charger; core tube adapter

and clamp with check valve and retrieval lines

attached; 2-10 ft. extension poles, 6.5 ft. (2

meter) lengths of 2” diameter core tube (CAB or

cellulose acetate butyrate polymer) with CAB core

catchers attached, 2” diameter PE (polyethylene)

end caps; duct tape, marker pens, portable drill

and 1/4” bit; tube cutter tool; glass or

polypropylene sample bottles; field crew of at

least 2.

A.1 Collecting the Core

1. Locate the sampling station with an

appropriate field positioning system that

provides suitable accuracy (± 6 to 15 ft.).

2. Measure the water depth using appropriate

means, such as a sounding line, marked pole

or fathometer.

3. Check for secure attachment of the retrieval

lines to the core tube mounting clamp.

4. Insert a 6.5 ft. length of 2” diameter CAB core

tube (core catcher end down) into the

mounting clamp and tighten the four wing nuts

securely by hand. Make sure clamp is

tightened evenly.

5. Choose an extension pole of appropriate

length (water depth or longer) and insert it into

the mounting plate socket; secure it using a

1/4” bolt and locknut.

6. Slip the flared lower end of the extension

tube over the check-valve end of the core

tube adapter, and hold it on by applying

upward tension on the retrieval lines. Lower

the system vertically (CAB tubing first) into

the water to the bottom. Press and

vibrate tube into the sediment until

it is inserted 6 ft., or until refusal

occurs. Note insertion length by

markings on extension pole.

7. Disengage the extension pole and

stow on board sampling vessel.

8. Retrieve the core tube containing

the sample by pulling on the two

retrieval lines, either manually, or

by using a davit mounted hand

winch.

9. With tube and barrel held vertically

in the boat, drill hole in tube just

above the top of the sediment

column to drain off water.

10. Cut off the tube just above the

sediment surface and cap both

ends.

11. Label the tube lengths with sample

station ID codes using a permanent

marker; make sure the upper ends

are marked as such.

12. Stow core within a cooler or

enclosed box with bag ice.

Transport ashore for processing as

soon as possible.

A.2 Processing the Core

The sediment core is usually processed

in a nearby field facility in order to

describe it's structure and create

subsamples for chemical analysis. This

is important to document the core

content and to maintain sample quality.

Both the 2” pole vibro-cores and the 4”

submersible vibro-cores, contained and

transported ashore in CAB plastic tubes

after sampling, are processed in the

same way. First, cut off, cap and tape

the cores in sections no longer than 48", and

preferably 40” (about 1 meter) in length. This

Ohio EPA Sediment Sampling Guide

length fits onto a stainless steel tray on the core

processing table, and can be photographed

conveniently in only three frames of film. Make

these core cuts with either a hacksaw or the

vibrating cutter tool described below. When sub-

sampling the core later on, take care not to

include any sediment from this cut surface, or any

plastic chips from the saw cut.

Next, cut the CAB core liner (filled with sediment)

lengthwise along opposite sides of the 40” section

(See Summary Diagram below, Step 1.). Note:

cut through the liner wall without cutting

significantly into the sediment core itself.

Disturbed sediment adjacent to the liner wall

should not be sampled anyway, but it is important

not to contaminate the undisturbed interior of the

core with plastic chips or other debris from the

cutting process. If, before coring, the outer wall of

the CAB liner (1/16” thick) is scored or pre-cut

halfway through with a circular saw or other tool,

then the final cut during processing can be made,

with a razor knife. However, CAB plastic is very

tough, and cutting with a razor knife can be

dangerous and difficult to control without cutting

into the core. The best hand tool available for

cutting hard plastic liners is an electrical vibrating

or "reciprocating" saw of the type used in industry

to cut sheet metal or in medical practice to cut off

plaster casts. When used with a blade guider the

cut depth can be controlled so as to barely cut

through the liner walls. The cuttings tend to form

ribbons rather than chips, which helps in avoiding

contamination of the sediment inside. Also, the

vibrating blade is much safer to use than a

conventional saw blade, since it does not readily

cut soft material such as skin.

Once the liner wall is cut through along opposite

sides (top and bottom of the horizontal core) , use

a flat, thin blade of rectangular shape to cut the

sediment core lengthwise into two half-cylinders,

using a series of vertical cuts along the core's

radial axis (Step 2, below). Vertical cutting in

discrete steps, rather than "dragging" the blade

through the core, insures that the layered

structure of the core is not obscured, and that

contaminants are not spread across layers.

Between each vertical cut, wash and scrub all

adhering sediment off of the blade in a bucket of

clean tap water. Note: it is usually not practical to

decontaminate the blade fully after each cut, but

any chance of contaminant carryover between

zones can be minimized by cutting through the

less oily parts of the core first, (it helps if the blade

is wet when cutting through oily silt or stiff clay

sediments, which tend to adhere). A cleanly cut

surface is best for documenting core structure.

Arrange the two half-cylinders of the core section

side-by-side, with the cut surfaces facing up (Step

3, below). Extend a tape measure along them,

starting at the original top end of the core.

Photograph the core in color with a track-mounted

35mm camera. With 160 watts (4, 4’ lamps) of

fluorescent light, 200 speed film is suitable for

good results. Insure that the wet surface of the

core does not reflect light directly into the camera

lens. A polarizing filter helps to reduce

reflectance off the wet core surface. Photograph

the core section in overlapping frames; place a

small label with core field ID number so that it

appears in each frame. Advance the tape

measure appropriately for any additional sections

of the same core. While the core section is still

intact record a general description of the core

structure, noting zones of different color

(consistent with the Munsell

color chart), texture,

sediment type (silt, sand, clay, gravel, etc.), and

apparent oiliness.

Collect each core interval, as pre-determined in

the study plan, from the undisturbed core interior

with a clean, stainless steel spoon or spatula.

Place the sediment from an individual core

interval into a clean stainless steel mixing bowl of

appropriate size (bowls and spoons are

precleaned according to Ohio EPA protocols).

Mix the sediment with a clean stainless steel

spoon thoroughly or until visually homogeneous.

During this operation, remove any obviously "non-

sediment" objects from the sample; bottle caps,

broken glass, sticks, large rocks, etc.

Place approximately 150 ml of sediment collected

from each core interval into a labeled 250 ml

wide-mouth glass jar (precleaned according to

Ohio` EPA protocols), leaving space at the top of

the bottle for later mixing (unless the samples are

for volatile organics analysis, in which case the jar

should be completely filled). Label each jar with

a unique station identification number, with a

suffix indicating the layer (X cm - Y cm) of the

Ohio EPA Sediment Sampling Guide

STEP 1

STEP 2

STEP 3

Blade

STEP 1

STEP 2

STEP 3

Blade

sample. Record a description of the layers in

each core on core Observation Log Sheets.

Store the sample bottles on ice or in a refrigerator

until transfer shipment to the analytical

laboratories.

Summary Diagram of Core Processing Steps

Ohio EPA Sediment Sampling Guide

APPENDIX B SEDIMENT OXYGEN DEMAND

APPENDIX B - Sediment Oxygen Demand

(SOD)

Sediment oxygen demand is a measure of the

oxygen consumed by biochemical decomposition

of organic matter in stream or lake deposits.

Sediment can be divided into two broad

categories, benthic and sludge according to Velz,

1970. Benthic deposits originate from runoff

containing detrital matter. These deposits are

characterized by Velz as "old compacted

accumulations of partially stabilized organic

residues and river muds". They are relatively

inactive, decomposing at a very slow rate.

Sludge deposits are described by Velz as "fresh

organic deposits arising primarily from current

municipal and industrial waste discharges".

These deposits undergo "active decomposition of

a semi-anaerobic character, with end products

readily leaching into the overflowing stream and

utilizing dissolved oxygen from that water.”

Sludge deposition is a result of settling and

therefore, a function of stream flow conditions and

particle size. Following a period of high stream

flow and accompanying scour, sediments should

be allowed sufficient time to settle and

accumulate prior to measuring their oxygen

demand. According to Velz, sludge deposits

resulting from a day or two of deposition following

a storm will have a negligible effect on instream

dissolved oxygen. It takes 40 to 50 days for

deposition of accumulated sludge deposits to

have a pronounced effect on the instream

dissolved oxygen. SOD sampling locations

should be in areas of extensive sludge deposits

that have large (> 100%) diurnal D.O. swings.

Procedures for the Large SOD Chamber:

C Measure and record the water velocity (2.4

inches) above the sediment surface.

C Calibrate the D.O. meter and measure and

record the surface D.O.

C Record the SOD chamber number.

C Insert the D.O. probe into the SOD chamber.

C Raise the chamber top and lower the entire

chamber into the water.

C Turn on the stirrer and verify proper operation.

C Adjust the rheostat to duplicate the measured

stream velocity at the site.

C Lower the respirometer to the bottom

with the top extended.

C The ammeter (located to the left of the

rheostat) displays the current in

amperes which is converted to water

velocity by using the graph in Figure 1.

Lower the chamber top to seal the

chamber. Record the water depth.

C Record the starting time and initial

D.O. concentrations. If a D.O. meter

chart is being used, the starting time

should be marked directly on the chart

paper.

C Manual readings should be taken

every five minutes and adjusted as

needed depending on the oxygen

uptake of the sediment.

C The readings are complete after D.O.

concentrations decrease by 2 mg/l or

after two hours (which ever occurs

first).

Procedures for the Small SOD

Chamber:

C Measure and record water velocity

measurements (2.4 inches) above the

sediment surface.

C Calibrate the D.O. meter. Measure

and record the surface D.O.

C Record the SOD chamber number.

C Place the chamber in sediments.

C If the sediments are disturbed, wait

several minutes for the sediments to

re-settle, then insert the D.O. probe

into the chamber.

C Make sure that no air is trapped within

the chamber.

C Turn on the chamber motor and use

the rheostat to regulate the velocity to

the measured stream velocity. Water

velocity within the chamber is shown

directly on the rheostat's dial.

C Install a second SOD chamber

adjacent to the first one and seal the

bottom with a plastic lid prior to

placement to exclude sediments from entering

the chamber. This chamber will be used to

measure the oxygen demand of the water

column. If only one SOD chamber is available,

use the D.O. change in dark productivity bottles

for water oxygen demand.

Ohio EPA Sediment Sampling Guide

C Record starting time and initial D.O.

concentration. If a D.O. meter chart is being

used, the starting time should be marked

directly on the chart paper.

C Manual readings should be taken every five

minutes and adjusted as needed depending

upon the oxygen uptake of the sediment.

C The readings are complete after D.O.

concentrations decrease by 2 mg/l or after two

hours (which ever occurs first).

Additional Data:

C surface incident light radiation using a

pyranometer

C light and dark bottle productivity

C water temperature

C surface and bottom water turbidity

C light reaching sediments (using a photometer

and submerged cell)

C sediment description and sample location; (see

data sheet)

C bathymetric survey results

C water samples for BOD

, cBOD

, COD and

Chlorophyll a

Calculations

SOD = 1.44 (V/A)(b

)

where:

SOD = Sediment Oxygen Demand in

g/m

/day

1.44 = conversion factor to convert to

g/m

/day

V = volume of chamber in liters

A = area of chamber in square meters (A

= Jr

)

= rate of D.O. change inside the SOD

chamber

= rate of D.O. change inside the

"blank" SOD chamber or dark

productivity bottles.

Results should be normalized to 20E C using the

following equation:

SOD

= SOD

/(1.065T-20)

where:

SOD

= SOD at original temperature in EC

SOD

= SOD at 20EC

T = Temp in EC

Ohio EPA Sediment Sampling Guide

APPENDIX C SAMPLES FOR SOLID PHASE SEDIMENT BIOASSAYS

APPENDIX C - Sample Collection for Solid

Phase Sediment Bioassays

Grab samples of sediment are collected using a

stainless steel dredge, corer, or scoop. A transect

or grid is established at each site and sediment is

collected from a minimum of three subsites. The

number of subsites/site will vary (e.g., depending

upon width of the waterbody, water flow patterns,

size and orientation of objects at the bottom,

depth of sediment). Aliquots of the top 10

centimeters (cm) from each station replicate

subsite are composited to form the site sample.

These aliquots should be as near the same size

as possible and thoroughly mixed prior to splitting

between containers for toxicity testing and

chemical analysis.

The mixing must produce a homogeneous

sample (i.e., uniform in color, texture, and

moisture content). Separate samples are

collected from reference sediment and sediment

of concern sites. One reference site may be used

with more than one sediment of concern site. The

concept of reference and sediment of concern

sites is somewhat similar to the upstream and

mixing zone samples, respectively, used in

effluent bioassays. The reference sediment is

similar (e.g., particle size, organic enrichment) to

the sediment of concern when previous physical

and chemical analyses are available to assist in

site selection. If the data do not exist, the

reference sediment and sediment of concern

should be collected from sites where it appears

that similar depositional patterns have occurred.

Location of the site selected for collection of the

reference sediment and overlying water is

dependent upon the purpose of the test and the

possibility of a point source or nonpoint source

affecting interpretation of results obtained with the

sediment(s) of concern. These guidelines are

based upon those contained in ASTM (1994).

Overlying Water Collection: Ohio EPA rearing

unit water is routinely used in the sediment

bioassay as the overlying water. The EPA

rearing unit water is carbon-filtered and oyster

shell-filtered Columbus city tap water that has

been aged at least 48 hours. This water is of an

acceptable

quality to support aquatic life as shown by its

routine use in our rearing units. Water

from the reference site collected for use

as overlying water for the sediments

used in the toxicity test may be used if it

better suits the project objectives.

Another source of high quality water

(e.g., further upstream or from a nearby

watershed) may be used if water from

the reference site is not available in

sufficient volume or is otherwise

unsuitable for use in a test.

Volumes of Sample Required and

Collection Containers:

Sediment should be collected from a

depth that will represent expected

exposure (U.S. EPA 1994). Aliquots of

sediment at each subsite are composites

in a stainless steel bucket and

thoroughly homogenized using a

stainless steel scoop. The sample is

transferred to labeled wide mouth

bottles. High density polyethylene

(HDPE) bottles are routinely used, but

glass bottles fitted with Teflon-lined caps

should be used if organic chemicals are

a concern. Two HDPE bottles each

containing 540 milliliters (ml) of sediment

are required for each site. Four 250 ml

glass bottles are required.

Overlying Water Samples (if Rearing

Unit Water is not Used):

Nine gallons of water are required to

overlay the sediments (three gallons per

each control, reference, and sediment of

concern) during the 10 day test. The

water is collected as grab samples and

poured into labeled 1 gallon linear

polyethylene cubitainers. The stainless

steel bucket used to collect the site

water is rinsed with site water prior to

filling the cubitainers.

Additional Information:

Samples may be collected during a

rainstorm but are not collected during flood

conditions. Headspace in the sample containers

is kept to a minimum. Bioassay sample

Ohio EPA Sediment Sampling Guide

containers are labeled with the sample source,

date and time of collection, and name(s) of the

collectors. The samples are routinely packed on

water ice in insulated containers for transport.

Samples for chemical analyses should be

collected in accordance with this manual from an

aliquot of the sediment sent to the lab.

All samples for solid phase sediment toxicity tests

are transported to the Ohio EPA Division of

Environmental Services in Columbus where they

are stored at 4EC prior to use in a test. Sample

storage time is kept to a minimum ( < 2 weeks)

prior to use in a toxicity test, and most tests are

initiated within 4 days of sample arrival.

Hyalella azteca Maintenance:

Culture Vessels - Hyalella azteca are cultured in

rectangular polypropylene pans. The start of the

Ohio EPA culture was obtained from Mark Smith

at the U.S. EPA EMSL-Cincinnati, Newtown,

Ohio facility in July 1992. U.S. EPA (1994),

EMSL-Cincinnati (1991), and methods described

by Brooke et al.(1993) are the basis of the Ohio

EPA culture and test methods for H. azteca.

The 5 liter pans are 12 inches long, 7.75 inches

wide and 5.125 inches in height. Pans are filled

to approximately one-half capacity with 2-3.5 liters

of rearing unit water. Aeration is supplied to each

pan by a small bore glass pipette connected by

plastic tubing to the oil-free lab air supply. Each

culture pan contains a sheet of non-bleached

paper toweling substrate for the Hyalella. The

Hyalella may utilize toweling as an alternative

food source. The toweling is replaced when it

degrades, generally each week. The pans are

not routinely covered. These culture vessels are

on racks in our rearing lab and receive a 16-hour

light 8-hour dark photoperiod. Luminescence

averages 1256 lux (range is 800-1530 lux).

Culture water is changed in each pan on Monday,

Wednesday, and Friday. When working with

mature adults and intermediate-sized subadults,

the water is changed by pouring old water through

stacked number 30 (0.60 mm mesh) or 40 (0.425

mm mesh) and number 60 (0.25 mm mesh)

stainless steel U.S.A. standard testing sieves

meeting ASTM E-11 specification. The number

30 or 40 sieve retaining the larger organisms is

then back washed with new water to flush these

larger adult or subadult organisms into a clean

culture pan. The number 60 sieve will retain any

new young. These newly-hatched animals of a

known age range are placed into their own culture

by backwashing the number 60 sieve directly into

a clean culture pan. The next time culture water

is changed, the two to three day old animals are

collected with a number 60 sieve and divided

between two culture containers of 300 animals

each to facilitate growth and diminish competition

for food. When the Hyalella reach 15 days or

older, too old for use in tests, young within seven

days of age are combined and 300 animals are

reserved for breeding purposes. If a reproductive

count is desired, the young in the number 60

sieve are first rinsed into a large glass culture dish

and counted on a lighted surface before being

placed in the new culture pan. Culture pans are

labeled with the age of organisms they contain.

To culture the younger animals, number 50 (0.30

mm mesh) and/or 60 sieves are used when

changing the water.

A glass pipette (3 mm bore size or greater) is

used to facilitate counting and transfer of the

juveniles. Any culture thinning or other handling

of the older organisms (adults or intermediate

subadults) requires a glass pipette of at least 5 to

6 mm bore size. Cultures are kept for

approximately 90 days then are discarded unless

needed for more production or

initiating/supplementing a back-up culture.

Feeding - The Hyalella cultures are maintained

on a diet of Cerophyl and Tetramin flake fish food.

Five grams of each ingredient are added to one

liter of deionized water. The amount of each solid

ingredient is weighed on a Mettler AE 163

balance. The mixture is blended for

approximately 4 minutes on a medium setting to

mix and chop up the food. Solids content of this

food is approximately 9.1 g/L + 10 % (range 8.2-

10 g/L). Feeding rate is 2.5 ml food per liter of

culture water. Typically, each culture pan

receives 5 ml of food solution once per day on

weekdays and for convenience, once per day on

weekends when toxicity tests are being

conducted. The stock food container is gently

agitated prior to each use and as needed during

feeding. The food container is stored in a

Ohio EPA Sediment Sampling Guide

refrigerator at 4EC between uses. Food not used

within a 30-day period is discarded.

The Ohio EPA Division of Environmental Services

should be contacted for revisions or updates to

the sediment bioassay procedures.

Ohio EPA Sediment Sampling Guide

APPENDIX D STANDARD SAMPLING FORM

APPENDIX D - Standard Sampling Form

Ohio EPA Sediment Data Collection Sheet

Project:_______________________________________________________________

Collection Date:______________________ Collection Time:__________________

Collector(s):__________________________________________________________________________________

Weather Conditions: ___________________________________________________________________________

Sample Location Description (Provide Diagram of Sampling Location(s) on opposite Side) :

Waterbody Name: _______________________________ River Mile Location: ________________

Latitude: _______________________________ Longitude: ________________________________

Sample Site Description: ______________________________________________________________

Ambient Site Information (water):

Conductivity _______________ Dissolved Oxygen _________________ pH ______________

Temperature _______________ Current Velocity _________________

Sediment Collection Information:

Water Depth Above Sample: _______________ Sediment Sample Depth: _____________________

Collection Device: Scoop ______ Eckman Dredge ______ Corer ______ Other ______

Sample Type: Grab ______ Composite: ______

Sample Replicate Collected? YES or NO Sample Duplicate Collected? YES or NO

Replicate ID/Name: _______________________ Duplicate ID/Name: _________________________

Sample Information:

Sediment pH (undisturbed) _____________ Sediment pH (post-homogenization) ____________

Color (Munsell Soil Color Chart Number): _________________________________________________

Texture (particle size description): ________________________________________________________

Odor: _______________________________________________________________________________

Additional Comments: _________________________________________________________________

Sand - Particles 0.06-2.0 mm in diameter, possessing a gritty texture when rubbed between fingers. Loose materials (not cohesive) that often

cannot be molded into shapes (non-plastic).

Silt - Particles 0.004-0.06 mm in diameter, generally fine material possessing a greasy or smooth, talc-like feel when rubbed between fingers.

Non-plastic and not cohesive.

Clay - Particles less than 0.004 mm in diameter, which forms a dense, gummy surface that is difficult to penetrate with tools (hardpan). Clay is

both plastic and cohesive.

Marl - Calcium carbonate, usually greyish-white, often containing fragments of mollusc shells.

Detritus - Dead, unconsolidated organic material including sticks, wood, leaves, and other partially decayed coarse plant material.

Peat - Partially decomposed plant materials characterized by an acidic pH; parts of plants such as Sphagnum moss sometimes visible.

Muck - Black, extremely fine, flocculant material composed of completely decomposed organic material (excluding sewage).

Sludge - Organic matter that is decidedly of human or animal origin.

Ohio EPA Sediment Sampling Guide

APPENDIX E SEDIMENT SAMPLING EQUIPMENT

APPENDIX E - Table of Sediment Sampling Equipment

TYPE MODEL CURRENT SUBSTRATE

TYPE

REMARKS ILLUSTRATION

GRAB Spoon

Scoop

Zero to

Slight

All C Use only in relatively calm and

shallow water.

C Relatively little sample

disturbance.

C Simple and inexpensive

C Fines may washout when

retrieved through water column

GRAB Eckman

(Birge)

Zero to

Very Slight

Clay and Silt C Use in relatively calm water.

C Pebbles and branches may

interfere with jaw closure

C Excellent jaw shape and cut.

C Relatively little sample

disturbance.

C Poor stability. Light weight

allows for tendency to “swim”

in a current. Sometimes

causes miss triggers.

C 0.02 m

sample area.

C Weight with sample is 10 kg.

GRAB Petite

Ponar

Peterson

Zero to

Very Slight

Clay to fine

gravel

C Need relatively calm/sheltered

waters.

C Good stability.

C Poor jaw shape and cut.

Sample disturbance.

C Less washout if extra weights

are used.

C More cumbersome than an

Eckman; requires a winch.

C 0.1 - 0.2 m

sample area.

C Weight with sample is 30 - 50

kg.

CORE Box Zero to

moderate

Clay to sand C Difficult to handle.

C Large sample size.

C Requires boat/barge with

winch.

C Rectangular shaped box.

Ohio EPA Sediment Sampling Guide

TYPE MODEL CURRENT SUBSTRATE

TYPE

REMARKS ILLUSTRATION

GRAB Shipek Zero to

strong

Clay to gravel C Requires boat/barge with

winch (mini shipek can be

used manually).

C One of the most reliable in

terms of triggering, stability,

washout, and leaching.

C Excellent jaw shape and cut.

Extremely clean cutting action.

C 0.04 m

sample area.

C Weight with sample is 60 - 70

kg (mini shipek weight with

sample is 20 - 30 kg).

CORE Manual Zero to

strong

Clay to sand.

Inserts

needed for

sandy

samples.

C Recommended for use in

shallow water.

C Deployed by hand or by driver

(hammer).

C Extension handles can be

used for deeper waters.

CORE Coring

Tubes

Zero to

moderate

Clay to sand.

Inserts

needed for

sandy

samples.

C Quick and easy.

C Relatively undisturbed sample.

C Small sample volume.

C Samples sometimes

compressed.

CORE Split

Spoon

Zero to

moderate

Clay to sand.

Inserts

needed for

sandy

samples.

C Recommended for use in

shallow water.

C Deployed by hand or by driver

(hammer).

C Vertical profile remains intact

and is visible.

C Point design can reduce

sample compaction.

C Stones can interfere with

collection.

C Equipment is heavy.

Ohio EPA Sediment Sampling Guide

TYPE MODEL CURRENT SUBSTRATE

TYPE

REMARKS ILLUSTRATION

CORE Gravity Zero to

moderate

Silts and

clays

C Recommended for rivers.

C Depths up to 10 meters

CORE Phleger Zero to

moderate

Silts C Good for short cores in soft

sediments.

C Quick and easy.

C Relatively undisturbed sample.

C Small sample volume.

C Samples sometimes

CORE KB Core Zero to

moderate

Clay to sand.

Inserts

needed for

sandy

samples.

C Quick and easy.

C Relatively undisturbed sample.

C Small sample volume.

C Samples sometimes

compressed.

In-situ SOD Zero to

moderate

Clay to gravel C For determining sediment

oxygen demand.

C Not for collection of sediment

samples.

Adapted from Environment Canada, 1987; Fay, 1987;Plumb, 1981

Ohio EPA Sediment Sampling Guide

APPENDIX F SEDIMENT SAMPLE VOLUME AND CONTAINER TYPE

APPENDIX F - Sediment Sample Volume and Container Type for Samples Submitted to the Ohio

EPA Division of Environmental Services Laboratory

Parameter Sample amount No. Containers Container Type

VOC's 60 mls by volume 1 Septum vial or 60 ml wide

mouth glass with Teflon lined lid

- fill to eliminate head space

BNA's 100 g 1 500 ml wide mouth amber glass

with Teflon lined lid

Pesticides/PCB's 100 g 1* 500 ml wide mouth amber glass

with Teflon lined lid

Metals 250 g 1 500 ml wide mouth glass with

Teflon lined lid or 500 ml HDPE

Nutrients 500 ml wide mouth glass with

Teflon lined lid or 500 ml HDPE

Bioassay 540 mls by volume 2 500 ml wide mouth amber glass

with Teflon lined lid. HDPE

may be used if organics are not

a concern.

Particle Size 500 g 1 Plastic “zip lock” bag or 500 ml

HDPE

All other samples (TOC, CN, etc.) 1 125 ml glass jar with Teflon

lined lid. One jar for all

remaining parameters.

* The analysis can be performed on an aliquot from the BNA container. Therefore, a separate container for

Pesticide/PCB analysis does not need to be submitted if a sample for BNA analysis is also submitted.

Ohio EPA Sediment Sampling Guide

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Ohio EPA Sediment Sampling Guide

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