DRAFT
CHARACTERIZATION OF SAMPLES
FROM HAZARDOUS WASTE SITE INVESTIGATIONS
U.S. ENVIRONMENTAL PROTECTION AGENCY
Region VII Laboratory
25 Funston Road
Kansas City, Kansas 66115
July 1981
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907D81002
In general , samples are taken as part of the investigation of hazardous
waste sites for various reasons including the following:
1. To determine if the wastes are hazardous as defined by Section 3001 of
the Resource Conservation and Recovery Act (RCRA). A waste is defined as
hazardous if it has the characteristics of ignitability, corrosivity,
reactivity, or toxicity; or if it contains certain specific chemicals; or
if 1t 1s from specific sources.
2. To determine whether the presence of a waste at a particular location
represents an "imminent" hazard requiring immediate corrective action.
3. To determine whether the waste represents a potential hazard requiring
eventual removal.
4. To characterize the material to determine an appropriate disposal
solution.
5. To determine the levels of specific components such as PCB's or dioxin.
Very specific and detailed tests have been provided to determine the RCRA
characteristics of ignitability, corrosivity, reactivity, and toxicity.
Further characterization procedures are not well documented.
The purpose of this report is to describe methodology and procedures which
characterize to the fullest extent practical samples taken from or near-
hazardous waste sites. The general objective is to identify and quantify
all components down to the 1% by weight concentration level for samples
taken directly from the site such as the contents of abandoned steel drums.
The desired concentration level for off-site samples such as leachate or
contaminated soil is generally 10 ppm. However, there may be occasions
where lower detection levels will be required for specific compounds.
It should be noted that these objectives may not always be achievable in
practice, especially for complex mixtures of wastes. Presently, there are
more than 5 million known chemicals. A comprehensive analytical approach
to identify and measure these chemicals does not exist. Such a task would
be incredibly complex and time consuming. The approach taken here is to
utilize established analytical methodology to measure components of current
environmental concern while attempting to achieve a reasonable mass balance.
Gross measurements such as total organic carbon will, therefore, often be
utilized.
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CHARACTERIZATION SCHEMATIC
Field
Characterization
Sample Delivered
to Laboratory
Review Field
Report
Open Sample and Record
Physical Observations
Perform Phase
Separations
Water Soluble
Liquid
Water Soluble
Solid
Water Insoluble
Liquid
Wate1- Insoluble
Solid
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Ignitability
per RCRA
Water Soluble
Liquids
v Corrosivity (pH)
per RCRA
Determine
TOC
Total Dissolved
Solids
IF LESS THAN
10.000 ppm - STOP!
IF LESS THAN
1% - STOP!
Purge & Trap
Scan (GC/MS)
IF NECESSARY
Cation Scan
ICAP
Neutral
Intractables
D.A.I.
Anion Scan
Ion Chromatograph
IF NECESSARY
V
Ionic
Intractables
M.A.S.
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Water Insoluble
Liquids
Ingnilability
per RCRA
V
Infrared Scan
Purge & Trap
Scan - GC/MS
Method 625
Type Scan
GC/MS - Capillary
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Ionic
Intractables
M.A.S.
Water Soluble
Solids
V
v EP Toxicity
""/ per RCRA
Percent
Moisture
V
Percent
Volatile Solids
V
TOC
IF LESS THAN
10,000 ppm
Anion
Scan
Ion Chromatograph
Cation
Scan
ICAP
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Water Soluble
Solids
EP Toxicity
per RCRA
Percent
Moi sture
Percent
Volatile Solids
V
Infrared Scan
Method 625
Type Scan
GC/MS - Capillary
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REVIEW FIELD OBSERVATIONS
The first and perhaps most critical step prior to in-laboratory
characterization is to review the field observations pertaining to a
particular sample. The analyst should then make a judgment as to what
analyses to perform, keeping in mind that the following step approach is
merely a guideline. For example, if the sample was taken from a drum
clearly labeled as ortho-chlorophenol (OCP), it would probably not be of
value to perform any tests except one for OCP. If a reasonable mass
balance is achieved (greater than 99% of the sample contents accounted for),
then additional work would not be useful.
In reviewing the field observations keep in mind that many of the tests are
merely screening methods which were not intended to be as detailed or compre-
hensive as in-laboratory methods. Carefully note any indications of unusual
hazards (e.g., cyanides, sulfide, caustics, acids, explosives) and plan the
laboratory procedures accordingly. Also plan for any low-level analyses which
may be needed. For example, the presence of 1 ppm of TCDD may be more signif-
icant than the 99.999% by weight OCP in the previously mentioned sample.
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DOCUMENTATION OF PHYSICAL APPEARANCE
The next step is to unpack the sample using standard laboratory safety
procedures (see Appendix A) and to document the physical appearance of
the sample. Specifically, note the number and types of phases, color,
viscosity, weight, an opacity. Although it is recommended that odor
observations not be deliberately made, any observed should be fully
described along with any other organoleptic responses (e.g., caused headache,
watery eyes, aftertaste).
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PERFORM PHASE SEPARATIONS
This step can be omitted if the sample is obviously a single-phase
homogenous system. Otherwise, it will be necessary to perform a phase
separation by .centrifugation or filtration as described in method 2. All
phases accounting for 1% or more of the total sample must be retained and
characterized separately.
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DETERMINE WATER SOLUBILITY OF EACH PHASE
The water solubility of each phase should be determined as described in
method 3. For the purpose of this characterization scheme, any phase
which is soluble to the extent of 1 g per liter of water is categorized
as water soluble. At this stage of characterization, the possible
categories are water soluble liquids, water soluble solids, water insoluble
liquids, and water insoluble solids.
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CHARACTERIZATION OF WATER SOLUBLE LIQUIDS
A water soluble liquid will very often contain large amounts of water.
However, occasionally signifcant amounts (>1% by weight) of dissolved
materials may be present. This is determined by performing total organic
carbon and total dissolved solids according to methods 4a and 5b,
respectively. Further characterization will not be required if the TOC is
less than 10,000 ppm and the IDS is less than 1% by weight.
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CHARACTERIZATION OF WATER SOLUBLE LIQUIDS (TOC >10>000 ppm)
Dilute the sample and perform a purge and trap analysis per method 6a.
If the TOC can be accounted for, then further characterization is
unnecessary. Otherwise, perform analyses for neutral intractables
(e.g., methanol, acetone) by method 7a and ionic intractables (e.g.,
formates, acetates) by method 8a.
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CHARACTERIZATION OF WATER SOLUBLE LIQUIDS (>1% by weight IDS)
Perform cation characterization by method 9a. Perform anion
characterization by method lOa.
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CHARACTERIZATION OF WATER INSOLUBLE LIQUIDS
This category would include many petroleum derived products such as fuel
oil, benzene,,gasoline, crude oil, and crankase oil. An infrared scan
should be done according to method lla to determine the types of functional
groups which are present. Further characterization should be performed on
dilutions following methods 6b (purge and trap) and 12a (GC/MS scan of
methylene chloride solution).
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CHARACTERIZATION OF WATER SOLUBLE SOLIDS
Ths category would include many inorganic and low molecular weight
organic salts. The first step is to determine the water or moisture
content of the. solid using method 13a. The percent of volatile solids
should be determined using method 14a. Other tests to be performed
Include a cation scan (method 9b), an anion scan (method ), and TOC
(method 4b). If the TOC result is greater than 10,000 ppm, further
characterization of ionic intractables (method 8b) should be performed.
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CHARACTERIZATION OF WATER INSOLUBLE SOLIDS
This category would include high molecular weight organics, polymers,
plastics, many man-made objects and debris, and insoluble salts. The
first step is to determine the water content or percent moisture
(method 13b) and percent volatile solids (method 14b). An infrared scan
(method lib) should be performed on a KBr pellet. Further characterization
Includes TOC, TOX, and GC/MS scan on methylene chloride extracts by
methods 4c, 5a, and 6b, respectively.
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