United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
&EPA
DIRECTIVE NUMBER:
TITLE:
OSWER 9951.1
TRANSMITTAL OF THE FINAL WASTE OIL INTERIM
ENFORCEMENT GUIDANCE DOCUMENT
APPROVAL DATE: DEC. 30, 1986
EFFECTIVE DATE: DEC. 30, 1986
ORIGINATING OFFICE: OWPEE
E1 FINAL
D DRAFT
LEVEL OF DRAFT
S"A — Signed by AA or DAA
D B — Signed by Office Director
DC — Review & Comment
REFERENCE (other documents):
SWER OSWER OSWER
DIRECTIVE DIRECTIVE Dl
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' no Atts cnvroflffiofltfl roection ooncy
Washington, DC 20460
QSWER Directive Initiation Request
1. Directive Number
9951.1 OSWER
2. Originator Information
Name of Contact Parson
BRUCE POTOKA
Mail Code
OS-520
Office
Telephone Code
382-2270
3. Title
TRANSMriTAL OF THE FINAL WASTE OIL INTERIM ENFORCEMENT GUIDANCE DOCUMENT'
4. Summary of Directive (include bnei statement of purpose)
The purpose of this document is to provide information to the Regions about the
technology of the waste oil industry as well as strategies for enforcement.
S. Keywords
Waste Oil Interim
6a. Does This directive Supersede Previous Directive(s)?
X No
b. Does It Supplement Previous Directlve(s)?
X No
Yes What directive (number, title)
Yes What directive (number, title)
7. Dratt Level
A-SignedbyAA/DAA
B - Signed by Office Director
C - For Review & Comment
0 - ii Development
8. Document to be distributed to States by Headquarters?
*-i- .
Yes
JL
No
This Request Meets OSWER Directives System Format Standards.
9. Signature of Lead Office Directives Coordinator \
MfrjiL+J^ '/ft, J^^^^
1 0. Name and Title of Approving Official
Date
4/6'7/fo
Date
EPA Form 1315-17 (Rev. 5-87) Previous editions are obsolete.
OSWER OSWER OSWER O
VE DIRECTIVE DIRECTIVE DIRECTIVE
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
OSWER 9951.1
DEC 3 0 1986
MEMORANDUM
SUBJECT: Transmittal of the Final Waste Oil Interim
Enforcement uidance Document
FROM: J". Wins ton /Porter
Assistant -'Administrator
TO: Waste Management Division Directors
Regions I-X
The Office of Solid Waste and Emergency Response has developed
the Waste Oil Interim Enforcement Guidance Document. The purpose
of this document is to provide information to the Regions about
the technology of the waste oil industry as well as strategies
for enforcement.-- Waste oil is a very complex environmental
issue owing in large part to the difficulty of tracing waste
derived fuels through a complex system of waste oil dealers.
The guidance was developed to assist those enforcing the waste
oil regulations to better understand the important issues. It
is interim guidance because the regulations for used oil management
have not been completed. As the regulations become complete or
changes in policy or technology occur, the document will be
amended accordingly.
*
The guidance document has been developed with the cooperation
of the Headquarters offices, Regions, and the National Enforcement
Investigation Center. Any questions regarding the document may
be directed to Bruce Potoka of the Office of Waste Programs
Enforcement (WH-527) FTS 382-2270.
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301986
"ASTE OIL INTERIM
ENFORCEMENT GUIDANCE
December, 1986
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Table of Contents
I. Introduction
II. Legal Authority and Site Entry
III. Summary of the Rule
IV. Enforcement Approach
V. Pre-insoection
VI. . Site Inspection
VI. Sampling
VII. Analytical Methods
IX. Glossary
X. Aooendices
A. Industry Practices for Used Oil Processing for
Fuels and Lube Stock
3. Regulatory Provisions
1. Effective Dates
2. Invoice System
3. Required Notice
C. Checklists
D. Sampling Protoleum and Petroleum Products; ASTM
Standard: 2546
E. PlKaging, Marking, Labeling and Shipping of Samples
•^
F. Lubricating Oil Additives; and Concentration of
Potentially Hazardous Constituents in Used Oils
G. Final Rule: 50 FR at 49164 to 49211 November 29, 1985.
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OSWER 9951.1
Introduction:
The purpose of this document is to provide technical guidance
to enforcement officials for planning and conducting inspections
and case development related to standards for used oil and
hazardous waste intended for energy recovery. The information
contained in this guidance pertains to regulations currently in
effect and violations identified can be pursued with enforcement
action. The regulations were published in final form on November
29, 1985, 50 Federal Register 49164, and took effect on various
dates between December 9, 1984 and May 29, 1986. These standards
added Subparts D and E to Part 266.
The final regulations establish three categories of waste as
fuel: 1) hazardous waste fuel, 2) off-specification used oil
fuel, and 3) specification used oil fuel (see glossary for defin-
itions). Each category is regulated differently. The primary
purpose of the waste as fuel regulations is to prohibit the
burning of hazardous waste fuel and contaminated used oil in
non-industrial boilers. In addition, the rules place more
restrictions on the management of these fuels (when they are
destined for energy recovery) which have been essentially
unregulated until this point.
'•:
The pnQJttMd management standards were scheduled for
iS>
final publication in the spring of 1987. There will likely be a
delay in the promulgation of any additional standards. The
proposed management standards, however/ and the date upon which
they take effect, should be monitored in the future.
1
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OSWER 9951.1
Once the proposed regulations take effect, the Office of Waste
Programs Enforcement' will distribute a comprehensive Guidance
covering all the used oil regulations.
The information provided in the document is intended to
provide both procedural and technical guidance to enforcement of
the regulatory provisions, as well as a brief summary of the
regulations. It is likely that many situations will arise in the
field that this document will not adequately address. The intent
is to provide general guidelines and approaches in enforcement of
the used oil regulations.
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OSWER 9951 .1
Legal Authority
Section 3008 of RCRA provides EPA with authority to enforce
the RCRA regulations, including hazardous waste fuel and the used
oil regulations. Section 3008(a) authorizes EPA to issue an admin-
istrative order requiring immediate compliance and/or assessing
civil penalties for violations of Subtitle C. It also authorizes
'i
EPA to commence a. civil action for injunctive or other "appropriate
relief" or for civil penalties for such violations. Under section
3008(g), any person who violates Scotitle C is liable for civil
penalties of up to $25,000 per violation per day.
In addition, section 3008(d) provides for the imposition of
criminal penalties on any person convicted of violating certain
specified provisions of Subtitle C. Although used oil is not
currently listed as a hazardous waste, criminal penalties can
apply to violations associated with used oil not involving
hazardous waste. The amendments to the Solid Waste Disposal
Act that accompany the CERCLA reauthorization bill expand the
criminal authorities of Section 3008(d). (See Section 9008(i)
of the Superfund Amendments and Reauthorization Act of 1986.)
Section J007(a) authorizes EPA employees or representatives
^^Hf
to enter an ^fcablishraent and conduct an inspection, copy records,
and obtain samples for the purpose of enforcing the RCRA regulations.
This authority extends to any establishment believed to be generating,
transporting, storing or treating a Solid or Hazardous Waste within
the meaning of Section 1004 of RCRA (S261. Kb) ( 2) ( i )).
3
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OSWER 9951.1
Finally, section 7003 authorizes EPA to commence a civil
action to abate' an imminent and substantial endangerment to the
public health or welfare or the environment caused by the handling,
storage, treatment, transportation, or disposal of hazardous or
solid waste. A section 7003 action may be brought against any
person contributing to such endangerment. Because the provision
applies not only to "hazardous waste" but to "solid waste" as
well, and because used oil falls within the statutory definition .
of "solid waste," a section 7003 action could be brought to abate
an endangerment caused by used oil.
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OSWER 9951.1
Entry/Refusal;
In the event that a facility or owner/operator denies an
official the right of entry for an inspection, an Administrative
Warrant must be obtained through the Regional office. If it is
anticipated that entry will be denied, a warrant may be secured
prior to arrival at the facility.
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OSWER 9951.1
Summary of the Rule
The primary purpose of this rule is to prohibit the burning
of hazardous waste and contaminated used oil in non-industrial
boilers (e.g., residential boilers). In addition, it places
restrictions on the management of these fuels (when they are destined
for energy recovery) which have been unregulated until this point.
There are three types of fuel addressed in Part 266: hazardous
waste fuel; off-specification used oil, and specification used
oil. Subpart D deals with hazardous waste fuel and Subpart E
deals with off-specification used oil fuel and specification used
oil fuel. (see Figure I flow chart). For t.he purposes of this
summary, the provisions of the two subparts will be addressed
together.
Subpart D applies to hazardous waste fuel, defined as any
fuel that has been blended with a hazardous waste (listed or
characteristic). In the case of a used oil mixed with characteristic
hazardous waste, if the mixture continues to exhibit the characteristic
of the hazardous waste/ it is hazardous waste fuel. Alternatively,
used oil which exhibits a characteristic, but has not been mixed
with hazardou* waste, is not considered hazardous waste fuel.
When used ott^is mixed with a listed hazardous waste it is regulated
under Subpart D as hazardous waste fuel, and the specifications
for used oil (§266.40(e)) do not apply.
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OSUI-:R
FLOW CHART PART 266: WASTE AS FUEL
USED OIL
RECYCLED
LISTED
HAZARDOUS
WASTE
'(MOTE)
USED OIL
RECYCLED
ANALYZED
EXCEEDS
1000 ppa
TOTAL
HALOGEM
REBUTTABLE
PRESUMPTION
UNSUCCESSFUL
REBUTTAL
HAZARDOUS
WASTE FUEL
SUBPART 0
PART 266
SUCCESSFUL
REBUTTAL
USED OIL
RECYCLED
ANALYZED
BELOW
1000 ppm
TOTAL
HALOGEN
(NOT MIXED
WITH H.W)
USED OIL
RECYCLED
SUBPART E,
PART 266
SPECIFICATION
ANALYSIS
OFF SPEC
USED OIL
FUEL
SUBPART E,
PART 266
SPEC USED
OIL FUEL
NOT
REGULATED
CIIKK
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OSWER 9951 .1
Note:
1. Used oil mixed with hazardous waste, exhibiting a characteristic
is regulated as a used oil if it no longer exhibits characteristic
under Part 261.
2. Hazardous waste from conditionally exempt small quantity generators,
less than 100 kilograms per month, mixed with used oil is regulated
as a used oil. §261.5(j)
3. Use oil mixed a hazardous waste from generators of 100 to 1000
kilograms of hazardous waste per month is a hazardous waste
except as Note 1 applies.
4. Used oil that exhibits a characteristic of hazardous waste is
regulated as used oil fuel provided it has not been mixed with
hazardous waste and it is recycled for energy recovery.
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OS'./ER 9951 . i
Subpart E applies to used oil and hazardous waste mixtures
not otherwise covered by Subpart D. The provisions under Subpart
E focus primarily on the prohibit ion- on burning, marketing standards
and recordkeeping. The specification established in Section
266.40(e) sets maximum levels for certain metals and total
halogens, and a minimum flash point. This is used to distinguish
used oil that -nay be burned in non-industrial units versus used
oil that must be burned in industrial burning units (spec and
off-spec used oil/ respectively).
Once an owner/operator claims and shows the specifications
for metals, total halogens and flash point are met and sells
it, the oil is no longer subject to used oil regulation. If
contamination levels in the oil are subsequently found to exceed
the specs, the oil is regulated under Part 266.
The following discussion describes each of the regulatory
provisions and their applicability. Each provision is explained
separately as it applies to the fuel type independ of the subpart
in which it is contained.
Rebuttable Presumption
A provision intended for distinguishing fuel types is the
rebuttable presumption, §266.40(c), established for total halogens
in used oil.j^iis provides a criterion (1000 ppm total halogen)
for presuming^hat a used oil has been mixed with a halogenated
hazardous waste. Therefore, in the event that there is'no other
information indicating used oil has been mixed with hazardous
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CSWER 9951.1
waste, the rebuttable presumption can be applied to make an
.initial determination. Although, if mixing with hazardous waste
is known to have occurred and supporting evidence confirms this
fact, then use 'of the rebuttable presumption is not neccesary
or appropriate.
The rebuttable presumption quantifies the mixture rule.
Used oil exceeding 1000 ppm total halogen is presumed a to have
been mixed with halogenated hazardous wastes (e.g., chlorinated
solvents). The level was specified at 1000 ppm total halogens
to provide an objective test for assuming mixing with hazardous
waste has occurred. If the total halogen level exceeds 1000
ppm, the burden of proof shifts to the owner to prove to the
Agency that the used oil has not been mixed with hazardous waste.
Because it is a rebuttable presumption, the owner/operator
may provide (and is entitled to provide) evidence proving that
the used oil exceeding 1000 ppm total halogens was not mixed
with a hazardous waste. (The burden of proof is on the owner).
In addition, however, if no listed halogenated solvent is present
at significant levels (i'.e., 100 ppm or greater), then it may
not be reasonable to presume mixing of hazardous waste with the
used oil. This reasoning is not necessarily true for all halogenated
-T
compounds, jjgt example, if chlorinated pesticides listed in
§261.33 are found at low levels (100 ppm or less) it may still
be reasonable to assume mixing has occured. In order to presume
mixing, however, the total halogen level must exceed 1000 ppm.
»
Therefore, even if "significant levels" of listed hazardous
waste are found, but the aggregate concentration of halogens is
below 1000 ppm, mixing must be proven by the Agency, not presumed.
10
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OSWER 9951.1
Notification
Part 266 also extends the notification requirement of RCRA
section 3010 to marketers and burners of hazardous waste fuel and
used oil fuel. The requirement applies to; marketers and burners
of hazardous waste fuel and off-specification used oil fuel, and
marketers and burners of specification used oil fuel who are the
first to claim their used oil meets the specifications and is,
therefore, unregulated. Such marketers and burners are required
to notify EPA of their waste fuel activities, providing the
information required by Form.EPA 8700-12 (Rev. 11-85) Notification
of Hazardous Waste Activity (use of the form is not mandatory),
and to obtain an EPA identification number. If a marketer or
burner already has an EPA identification number, he must still
notify EPA of this waste fuel activity. In addition, facilities
receiving hazardous waste fuel or used oil fuel must provide the
supplier with a "required notice" certifying that they have
notified EPA of their activity and have received and EPA identif-
ication number. Marketers and burners of hazardous waste fuel
and off-specification used oil fuel must also include in their
required notice a statement certifying that the fuels will be
burned only in industrial boilers and furnaces.
A facility that markets a used oil and claims it meets the
'*£
specif icatioir under $266.40(e) must provide evidence to support
this claim. Marketers of specification used oil fuel are only
subject to notification requirements if they are the first to
*
identify a used oil as specification oil. Therefore, if a
facility receives used oil not shown to meet the specifications,
the facility is subject to notification requirements.
11
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OSWER 9951.1
Analysis
Used oil is assumed to be off specification as generated
until a marketer or burner provides evidence for the first time
showing that it is in fact specification used oil fuel. This
determination must be made before any used oil can be burned in
a nonindustrial furnace or boiler and the determination must be
made for each shipment. (i.e., the prohibition requires that
only specification used oil fuel be burned in a nonindustrial
furnace or boiler §266.41). (Noted: Space heater exemption,
5266.41(b)(2)(iii))
The first marketer or burner to claim that his used oil
meets the specifications, and is therefore unregulated, must
perform analysis and maintain records to prove the specifications
are in fact met. This rule does not provide any guidelines for
frequency of analysis nor does it specify analytical methods to
be used. There are recommended methods in the preamble:
Analytical Testing to Demonstrate Compliance with Specification
Levels an the Rebuttable Presumption. A copy of the Recommended
Analytical Procedures (Table 6) is below. Additional methods
have been evaluated by the Office of Solid Waste and a report is
available explaining those methods. (Contact Paul Friedman in
the Office ofeSolid Waste (FTS 382-4796) for copies of the
m
document.) ^jf
Transportation
Transportation requirements for hazardous waste fuels are •:!-.•
RCRA Part 262 standards applicable*to generators of hazardous
waste and Part 263 standards applicable to transporters of hazar-!
12
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OSWER 9951.1
waste. Therefore, a manifest must be used for hazardous waste
£--el snipnents. An invoice must be used for off-specification
used oil shipment. The invoice does not necessarily have to be
-carried by the transporter, and the invoice need only be held on
file at the shipping and receiving facilities. (Specific inform-
ation requirements are provided in Appendix B). Effective since
March 31, 1986, these requirements supercede the warning label
requirement in the statute.
Used oil that meets the definition of combustible liquid
(Flash point below 200°F and above 100°F) and flanmable liquid
•
(Flash point below 100°F) is subject to Department of Transportation
(DOT) regulation at 49 CFR Parts 100-177.
13
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OSWER 995L .1
TA3LS E **
RECOMMENDED ANALYTICAL PROCEDURES
Parameter •
Total Halogens
Flash Point
Method
Source
Arsenic
Cadmium
Chromium
Lead
0808-81
1010
Preparation
3040*73050
3040*73050
3040*73050
3040*73050 .
ASTM
SW-846 and Proposed
Test Methods for
Evaluating Solid
Waste*
Determination
7060
6010
7131
7131
6010
7191
7191
6010
7420
7421
n
w
it
n
it
Notes: *Recommended only for non-sedimentaceous oils -t-SW-846
(Test Methods .for Evaluating Solid Waste) is available
from the U.S. Government Printing Office. Proposed Test
Methods for Evaluating Solid Waste is available from
NTIS under order No. PB8-103-026.
**Takl* 6 (50 FR 49189, November 29, 1985)
' "
14
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Recordkeeping
Records of transactions must be maintained at a facility Cor
three '/ears following the last transaction with another facility.
Part 262 and 263 record keeping and reporting requirements apply
to hazardous waste fuel generators and processors. Additional
records that must be maintained are the analyses, off-specification
fuel invoices, and required notices certifying notification.
Also, the first individual to market used oil as meetina the
specification (§266.40(e)) must maintain basic invoice information
with a cross reference to the analysis done for each shipment.
Storage
Marketers storing hazardous waste fuel .are subject t-o full
regulation under RCRA (including Parts 262, 264, 265 and 270).
3urners of hazardous waste fuel fall into two categories: existing
storage facilities and new storage facilities. The storage
requirements for existing facilities are Subparts A through L of
Parts 265, 270 and 124. An existing facility is any storage
facility in existance prior to May 29, 1986. New storage facilities
are subject to Subparts A through L of Parts :264, 270 and 124.
Mew facilities are not eligible for Interim Status storage of
hazardous waste fuel. Final permitting of existing hazardous
.waste fuel b^Ktng facilities will not be required 'prior to the
promulgation of the burning standards at which time one permit .
for both storage and burning can be issued.
15
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OSWER 9951.1
Finally, Spill Prevention Control and Counter-Tit asure Plan
v'SPCC Plan) storage requirements nay apply to these facilities
regardless of fuel type.
Statutory Requirements
Road oiling (Dust supression) using a hazardous waste or
hazardous waste mixtures is prohibited under section 3004(1) of
RCRA. However, used oil (and other solid waste) that is considered-
hazardous waste only because it exhibits the characteristic of
ignitibility is exempt from this prohibition.
Proposed Rules
Additional standards were proposed on November 29, 1985,
and the Agency is currently drafting burning standards for the
burning of hazardous waste fuel. These standards are often
referred to by several terms, such as, used oil, burning and
blending or wastes as fuel standards. There are four separate
rulemakings associated with used (waste) oil:
1. Burning and Blending (wastes-as-fuel) Phase I -
Final 50 FR 49164 (November 29, 1985.)
2. Listing Used'Oil - Proposed 50 FR 49258
(November 29, 1985.) .
3. Used Oil Management Standards - Proposed 40 FR 49212
^November 29, 1985.)
4. Spurdous Waste Fuel Burning standards - Draft (Burning
fanderds for Industrial Boilers and Furnaces)
The proposed rules would establish additional requirements
for recycled used oil prior to its burning as specification or
off-specification fuel. Therefore, enforcement staff should
monitor this development to discern any additional requirements
which come into effect as a result of future promulgation.
16
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OSWES 9951.1
Enforcement Approach
This next section provides an overview of the characteristics
of the regulated community and an approach to developing an
enforcement and compliance monitoring program. Although the
strategy and priorities selected by the Regions and States will
,1er>end on the nature of the market and the community in their
regions, basic priniciples will commonly apply.
In establishing an approach to the enforcement of these
provisions, it will be useful to understand the. structure and
onerations of the used oil management system. (see figure 2
flow chart). A basic factor to consider is the number of facilities
or handlers involved. It is estimated that there are many hundreds
of thousands of used oil generators and many hundreds of independent
collectors (or scavengers) of used oil. It is estimated that
there are approximately 200 to 250 processors or recycling facilities.
On the user end, there are several thousand fuel oil distributors
and thousands of burners. (Estimates indicate there are approximately
1000•industrial burners). Furthermore, there are many outlets f>-
used oil such as road oiling or asphalt processing,, other than
burning. Therefore, as the used oil is recycled and moves through
the systen,tthere is a bottle-neck (pinch point) at the process:-.:
JF
and re-reftiring facilities. (Included in the Appendix A is a
paper describing the treatment processes most commonly applied t -
used oil).
The universe of waste as fuel marketers includes fuel oil
dealers who operate as virgin fuel oil distributors. Because
17
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CSWER 9951.1
investigations may reveal that a virgin fuel dealer, is violating
their contract, this information should be made available to the
involved parties upon request. However, the mixing of waste
fuels with virgin fuel oil is r.ot orohibitad nor discouraged by
the Agency provided the fuels are managed in accordance with EPA
regulations.
The Regions, over time, will develop an understanding
of the management system as it operates in their states from the
notification forms, State and Regional inspection reports, and
communication with the regulated community. Furthermore, any
records of analysis of materials at these facilities may be
accessed by authority of Section 3007 (see Legal Authority).
This pertains not only to records required by requlation but any
records regarding the solid or hazardous waste generated or
stored on that site. (In many cases, a warrant may be necessary
depending on the nature of the investigation and facility history.)
The information from these efforts will be useful in both future
enforcement efforts, and the Agency's rulemaking efforts. For
these reasons and others, it is important that the initial
inspections be as thorough and effective as possible. Inspections
need to be designed to obtain information regarding overall
management practices, treatment processes and marketing practices
in the induaflpg-.
This Guidance provides an approach to selecting the points
in the system to target for inspection and in turn provide direction
for the inspection. The principal area for inspections to focus
on is at the used oil processing (marketing) facilities.
13
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HW
GENERATORS
-550,000
t
HW
HW
TRANSPORTERS
-700
KEY
HW - POTENTIAL ENTRY POINTS
FOR HAZARDOUS WASTES
HW
VIRGIN FUEL
OIL DEALERS
thousands
i
RECYCLERS
PROCESSORS
-240
• REREFINERS
-10
DISPOSAL OF
WASTE
STREAMS
OSWI-.K
HW
HW
INDUSTRIAL
BURNERS
-1,000
NON-
INDUSTRIAL
BURNERS
-90,000
FIGURE 2. USED OIL MANAGEMENT SYSTEM
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OSWER 9951.1
T^.ere are several reasons for focusing attention on these facilities:
1) the rule provides for more substantial requirements at this
point in the management system; 2) these facilities are the
fewest in number and largest in the volume of oil handled; and
3) they will have large networks of other handlers to which
materials cart be tracked. Essentially, these facilities are the
critical link in the movement of used oil from points of generation
to the end user.
The basic objective behind this approach is to bring the
marketers into compliance. Once this is done, burners also will
more easily comply with requirements as to the fuel type burned.
By focusing efforts on the large volume used oil processors
initially, the inspections will likely have the most impact and
provide information for subsequent targeting decisions. Obviously,
it may be necessary to target burners and generators for inspections
in order to substantiate information obtained at a marketer's
facility*
**^
(Mote, manyJ^plependent collectors also market used oil, although
t
they may not treat the oil. These are relatively large .volume
handlers that may have storage tanks for accumulation prior to
marketing.)
20
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OSWER 9951.1
In the following discussion several scenarios of violations
are presented to provide examples of situations likely to occur.
MARKETING/PROCESSOR FACILITY INVESTIGATION:
Markecer/processing facility violations will likely fall
into two categories:
o Fuel marketing violations
o Facility operating (Hazardous Waste) Violations
An example of the first type of violations is presented
below, and as shown, the burners may be involved in the activity.
If a marketer ships off-specification fuel or hazardous
waste fuel to a burner indicating that fuel has been supplied to
an industrial burner:
o Determine if the marketer has the required notice from
the burner certifying it to be an industrial burner.
o Determine if the burner notified.
If the Agency does not have a notification from the burner or if
there is uncertainty as to the type of burning facility, an
inquiry should be made as to the type of unit burning the fuels.
In the event the burner is using these fuels in a non-industrial
unit, further investigation and enforcement action should be
pursued:
o DBwrmine if the burner had knowledge of the fuel type
supplied by the marketer.
o A sample of the fuel supplied by the marketer to the
burner should be taken from the burner's facility,
when possible.
In this case, the marketer is definitely in violation if
the fuels have been marketed to a non-industrial burner. If the
marketer did so because of false information provided by the
21
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OSV7ER 9951.1
burner, action against both facilities may be pursued. Conspiracy
is a possibility in this situation, and should be considered
during an investigation. If, on the other hand, the burner
assumed the waste fuel was specification (as defined by 266.40(e))
and had not provided information identifying his facility as an
industrial burner, then only the marketer is in violation. This
type of violation is one of the more serious violations addressed
by this rule.
Industrial burne'rs that fail to notify EPA or fail to supply
the required notice to the marketer, but continue to burn off-
specification used oil fuel are in violation of the regulation.
In addition the marketer of the off-spec fuels is in violation of
the required notice - provision. The case-soecific factors should
be considered in assessing the severity of the violation, however.
In the case of burning hazardous waste fuel without, proper notifi-
cation, however, a more serious violation has occurred. The
burner is subject to hazardous waste storage standards and will
soon be subject to burning standards.
Investigating facility operating practices is a second area
of potential violations on which to focus. Hazardous waste
management violations, for example, treatment, storage and disoos.-?
of hazardous *faste without a permit may be common. Insufficieri
tr
secondary conrfwinment or diking required by SPCC Plans is another
example. In addition, these facilities may violate their wastes-..
discharge or pretreatment requirements depending on the type of
waste being processed for fuels.
22
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)SWER 9951.1
Establishing a case to prove such activity could require an
extensive records search and review, and a substantial sampling
and analysis plan. If illegal disposal of hazardous waste is
suspected, possibly through citizen reports, employee reports or
through sample analysis, then a preliminary step is to examine
records of shipments received to identify potential generator
sources, and an indication of the materials received. Several
states do require that used oil shipments be manifested by the
transporter or recycling facility from the generators. Therefore,
any state files should also be accessed.
Sampling incoming shipments and storage tanks will be necessary
to support case development. In some cases/ the sampling should
be done without advance notice to avoid alerting the facility
and potentially losing evidence. A facility that is accepting
hazardous waste will be prepared to redirect trucks in route,
transfer materials between tanks and between facilities given
sufficient warning. When sampling tanks, have the facility
owner/operators identify feedstock, processing and- product tanks,
and if possible, obtain a facility layout indicating this information.
This will baeuseful/ if not essential, in developing a case if a
violation i^touifd. In addition, records and other information
regarding outgoing shipments of the waste fuels should be obtained
to identify receiving facilities.
An investigation of a processing facility needs to be thorough
in order to identify questionable activity. In addition to
23
-------
OSWER 9951.1
reviewing records and samoling, examine'the equipment and the
treatment processes used at a facility. For example, if a processor
is accepting white-waters (i.e., oil-water emulsions often having
98% water) and claims to be separating the oils, determine if
the facility actually has the capability to break the emulsified
liquid to separate the oil. A large volume of materials of this
type can be handled and discharged in absence of any recycling.
The discharging of these materials in sewers or waters by themselves
may violate an NPDES permit or general pretreatment provision.
In addition, this activity can provide effective means of disposing
of hazardous waste. Furthermore, the structural integrity of
tanks and piping should be examined to assess the potential for
release. Underground or covered piping, especially, should be
evaluated for releases. Confirm that covered piping has an
identifiable end point.
Selecting burning facilities for inspection may be necessary,
particularly non-industrial burners. Direct targeting of non-
industrial burner facilities for sampling of their fuel oil,
however, will be a more research intensive effort as compared to
an indirect approach (i.e., selecting burners on the basis of a
*-•
used oil proeeaaor or marketer's customer listings). Identifying
non-industrial burners could be done by selecting a portion of
the universe. For example, the universe can be divided into
private or government which further breaks down to commercial
and residential or federal, state and local. Arranging for
sampling during delivery will usually require the cooperation of
24
-------
the owner/operator of the burning facility.
Another aspect of targeting non-industrial burners involves
determining that the facility is receiving a used oil fuel. if the
selection of burning facilities is based on the fact that they
are supplied by a marketer that handles used oil or waste fuels
then there is reasonable assurance that the fuel delivered will
industrial burners at random, however, increases the chance that
the fuel will not be used oil, but virgin oil.
There are benefits to either approach, and this depends on
the objective of the investigation. 1) Selecting burners because
they are supplied by a particular used oil fuel recycler or other
fuel distributor allows the investigation to be focused on the
compliance of a marketer or related marketers. In addition, it
reduces some of the targeting work and clearly links the marketer
and burner. 2) A random selection of burners (independent of
their fuel source) may reveal fraudulent business practices by
fuel suppliers. This also may result in the identification of
other waste fuel marketers operating outside of the system.
The procedure in absence of direct evidence, to determine- if
a fuel oil is indeed used oil (or a mixture) is discussed in the
section titl«d "Analytical Methods". Strategies and techniques
$£
for sampling» truck at a delivery point are discussed in the
section titled "Sampling".
Finally, any one of the scenarios discussed and others may
lead to discovery of facilities s'uspected to be operating outside
of the regulatory system or other State and Federal laws. In
25
-------
OSWER 9951.1
these cases, surveillance may be necessary to adequately develop
a case with evidence. At this time, a criminal investigator
should be contacted to assess.the situation.
Pre-inspectipn;
The following section on pre-inspections is meant only to
provide an outline of the type and source of information that
will be useful in preparing for an inspection. There are numerous
activities associated with preparing for inspections that this
document does not address.
A. Information needs
o Facility processes
o Facility size
o Materials handled
o Location
o Compliance status
o SPCC Plan - guidance
3. Sources of Information
o Notification Forms: EPA Notification of Hazardous Waste
Activity
o Permit Applications: Part A and Part B
o Biennial Reports
* '•
o EPA infection reports
o CERCL^Tiles
o State inspection reports
o State Solid and Hazardous Waste Files
o Dun and Bradstreet Reports
26
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OSWER 9951.1
Additional information -nay be requested crom a facility when
inadequacies or inconsistencies are discovered in the facility
files. Authorities under section 3007 of RCRA can be used to
obtain this information.
It is recommended that the states be contacted reqardino the
history of facilities. In many cases the states may have on-
goinq investigations or have conducted investigations of the
facilities in question.
-------
OSWER 9951.1
Site Inspect ion
An inspection is the primary means to determine a facility's
compliance status. If violations have been committed, then it is
necessary to collect supporting evidence for enforcement action.
The following section identifies specific requirements that
apply to the regulated community. In addition to containing
the cite to each standard, there is a brief explanation of each
standard. This is followed by examples of specific violations
which may be identified during an inspection, and the evidence that
may be needed to support those findings.
Theso guidelines should be treated as such; the following in
no way covers all situations that may be observed nor all types of
evidence which may be needed to support a case. If specific
situations arise in which inspectors need further guidance, they
should contact the appropriate enforcement or legal counterparts,
particularly if an inspector suspects he has discovered possible
criminal action.
Storaqe retirements may include. Spill Prevention Control
and Countermeasure (SPCC) Plan provisions and RCRA hazardous
waste storag£. reauirements. Although an inspector doing a RCRA
3£-
inspection ni^r not intend to perform SPCC inspections or be
trained to conduct the inspection, he may note possible violations
and refer them to the appropriate office in the Region or State.
Finally, used oil processing facilities do generate waste
streams which should be evaluated. Waste waters and sludges are
generated as a part of most processor, and these may be hazardous
28
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OSWER 9951.1
wastes. An inspection should be designed to obtain as much
information as 'possible about the fuel product and waste treatment
processes. • This will aid in assessing facilities waste streams
and compliance status with other standards.
29
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OSWER .9951.1
Generator Standards: Subparts D and E (§266.32 and §266.42)
Generators are subject to Part 262 provisions for hazardous
tfasta that is used as a fuel or to produce a fuel. If a generator
markets the hazardous waste fuel to a burner, then the generator
is subject to §266.34 (marketer standards). A generator burning
hazardous waste fuel is subject to §266.35 (burner standards).
Generators of used oil are not subject to Part 266 standards
unless they market the used oil to burners or burn the oil. If
the generator markets the used oil to burners, then the generator
is subject to §266.43 (marketer standards). A generator that
burns used oil is subject to §266.44 (burner standards). Therefore,
violations associated with a generator of used oil would relate
to marketing or burning activities which are addressed in later
sections.
(1) Small Quantity Generators (Also see Fj* at 10146 March 24, 1986)
(a) Hazardous waste from conditionally exempt generators (less
than 100 kg per month) mixed with used oil is subject to used
oil fuel standards (Part 266, Subpart E) ^hen the oil is burned
•4*
for energy recovery. §261.5(j)
(b) Generators of hazardous waste betwen 100 to 1000 kg per
month affip treated as hazardous waste fuel generators subject
ifc.
to Part*W6, Subpart D. If the hazardous waste is mixed
with used oil, the same provisions for listed and characteristic
wastes apply as discussed earlier.
30
-------
)SWER
!2) Soac* Heaters (§266.4 1 (2)(iii)(A)(3)(C))
Off-specificati-on used oil mav be burned for enerav recovery
in space heater- provided that:
A) The heater burnea only used oil that the owner or operator
generates or used oil received by do-it-your selfers who
generate used oil as Household waste: . -
B) The heater is desianed to have a maximum caoacitv of not
more than .5 million BTU per hour; and
C) The combustion gases from the heater are vented to the
ambient air.
The notification reouirements do not aoply to generators burnina
used oil in soace heaters.
31
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OSWER 9951.1
Marketer: Hazardous Waste Fuel
Requirements
Cite
Standard
1. Prohibition
$266.31(a)
2. Notification
S266.34(b)
3. Storage
§266.34(c)
4. Off-site shipments §266.34(d)
Hazardous waste fuel should
be marketed to only those
facilities that have notified
EPA and have I.D. numbers,
and the fuel sold to burners
should be only burners that
have industrial furnaces or
boilers.
Under authority in Section
3010 of RCRA, a marketer of
hazardous waste fuel must
notify EPA arid obtain an I.I).
number (even if the facility
has notified previously of
hazardous waste management
act i vi ty).
Parts 262, 264, 265 and 270
apply. Generators that
remove the fuel before 90
days are subject to $262.34
prov isions.
Waste shipped off-site are
subject to generator stand-
ards (Part 262).
-------
OSWFJR 9951.1
5. Required Notice
§266.34(e)
A one time written notice
certifying that the receiving
facility has notified I-,PA ami
obtained an I.I), number. A
marketer must receive this
before initiating any ship-
ment, and a burner's notice
must indicate that the fuel
will be burned in an indus-
trial unit.
6. Recordkeeping
§266.34(f)
7. Transportation
§266.33
In addition to other records
requirements of Parts 262,
264 and 265, a marketer must
maintain copies of the certi
fyino notices for 3 vears
after the last transaction
with any given facility.
A marketer that also trans-
ports hazardous waste fuel
is subject to Part 263,
transporter requirements.
31
-------
OSUKH 99'3l .1
Marketers: ll.ixa rdous Waste l-'uel
Possible Violations
1. Marketing of hazardous
waste fuel to non-
industrial burners.
2. Failure to notify EPA
of their hazardous waste
fuel activity (even if
notification for other
hazardous waste manage-
ment activity has been
done) or obtain EPA
I.D. number.
3. Failure to comply with
storage requirements of
Parts 262, 264, and
265.
266.34(b)
266.34(c)
Supporting Evidence
Sample/analyzo out-going
shipments of used oil fuel
to determine if it is
hazardous waste fuel or
sample fuel at burners.
Determine destination of
fuel shipment, i.e., indus-
trial or non-industrial
burner facility or: other
marketer. Obtain copy of
manifests if available.
Check files (and EPA files)
to verify absence of noti-
fication/EPA I.D. number.
Check for compliance with
storage reguirements and
examine for leakage around
tanks. If leaking, obtain
sample of tank contents.
Obtain photos of any leakage
Document deficiencies.
Assure presence of adeguate
SPCC plan and Contingency
plan.
34
-------
OSUER 9951.1
Shipping hazardous waste 266.34(e)
fuel to a burner or.
another marketer prior
to receiving the required
notice from the receiving
facility.
Shipping hazardous waste 266.33
fuel or Wflptitfl without a
manifest of*'Inadequate
manifest (e.g., unsigned,
no I.D. number,
inaccurate.)
266.34(e)(2)
265.76
Re ce i v i ng a s h i pine n t
of hazardous waste
fuel prior to sending
a required notice to
the shipping facility
or accepting the ship-
ment without a manifest,
and failing to report.
Failure to maintain 266.34(f)
the records for the
specified time period.
Check files for absence of
the required notice. Docu-
ment presence of invoices of
previous shipment without
matching notice.
Verify absence of manifest
for hazardous waste fuel
shipment, or obtain copy of
manifest. Sample/analyze
shipment if possible.
Document receipt of a ship
ment without previously
notifying shipper or re-
ceiving a manifest. Obtain
sample/analysis of shipment,
if possible.
Check files to verify absence
of reguired records. List
missing documents and obtain
copies of inadequate docu-
ments.
8. Accepting hazardous
waste without Interim
Status or a Permit.
3005 KCRA
Document receipt of hazard-
ous wastes. Copy labels,
manifest or other information
indicating material is
hazardous waste. Photograph
containers. (Apply rebuttable
presumption for TX in used
oil). Sample/analyze to
confirm prsences of hazardous
wastes if necessary. Copy
invoices confirming shipment.
Sample/analyze receiving
facility to verify used oil
mixed with hazardous waste.
-------
OSWER 9951.L
Marketers: Used .Oi I Fuel - .Suhpart tl
Requirements
1. Prohibition
Cite
S266.41(a)
2. Analysis
S2f66.43(b)( I)
3. Notification
§266.43(b)(3)
4. Invoice System
S266.43(b)(4)
Standards
Off-specification used oil
fuel may be marketed to
only facilities that have
notified EPA and obtained
an I.D. number, and to
burners that burn the fuel
in industrial furnaces or
botiers.
A marketer of used oil must
have analyses or other infor-
mation documenting a used oil
meets the specifications of
§266.40(e) prior to selling
it as spec-used oil.
A facility must notify EPA
of the used oil fuel acti-
vities regardless of prior
notification of hazardous
waste management*
A marketer must prepare an
invoice for any shipment of
off-specification used oil
and provide the specified
information to the receiving
facility (see appendices).
-------
OSWKR 9951.1
5. Required Notice
S266.43(b)(5)
6. Recordkeeping
S266.43(b)(6)
A one-time written notice
certifying that a receiving
facility has notified L'PA
arid has an I.I), number for
handling or burning off-spec
used oil fuel. Burners must
certify that off-spec used
oil is burned in industrial
units.
Invoices (and invoice infor-
mation for spec used oil
shipments) must be maintained
for 3 years after the last
transaction with any given
faci1ity.
17
-------
OSWER 9951.1
Marketers:. llsud Oil l-'ue 1
Possible Violations
1. Marketing off-speci-
fication used oil to
non-industrial burners
266.41(a)
2. Failure to provide
sufficient analysis or
other information
proving a used oil
meets the specifi-
cations, and marketing
to non-industrial
burners.
3. Failure to notify the
Agency of their used
oil fuel activity or
obtain I.D. number.
4. Failure to properly
invoice off-specifi-
cation used oil.
5. Shipping off-specifi-
cation used oil to a
burner or another
marketer prior to
receiving the required
notice from the
receiving facility.
266.43(b)(1)
and (2)
266.43(b)(3)
266.43(b)(4)
266.43(b)(5)
Supporting Evidence
Document shipments to non-
industrial burner. Obtain
copies of invoices. Obtain
copy of analysis. Sample
oil when possible.
Document shipment to non-
industrial burner. Obtain
copy of invoices.
receiving facility
industrial burner.
Document
is a non-
Obtain
copy of analysis
def iciencies.
and document
Check files (and EPA files)
to verify absence of notice
and/or I.D. number.
Document inadequacy of
invoice information. Obtain
copy of invoice.
Obtain copies of invoices
and the required notice.
Copy to illustrate receipt
after shipping. Document if
notice is not on file or
never received.
3H
-------
OSWI:R 9951.1
Possible Violations
Ci te
6.
Receiving a shipment
of off-spec fuel prior
to sending a notice to
the s' ' ' A«"-L,....
266.43(b)(5)
7. Not maintaining the
necessary records for
shipment of specifi-
cation used oil fuel.
266.43(b)(6)
Check files (and shipper's
files to verify absence of
required notice or invoice
or obtain copies or notice
and invoice showing receipt
of shipment prior to notice.
Check files to verify absence
of required records. List
missing information in files.
Obtain copies to illustrate
inadequacies. Note owner/
operator responses to
questions concerning record-
keeping.
39
-------
OSWER 9951.1
Uurners: Hazardous Was«« Fuel
Requirements
1. Prohibition
2. Notification
Cite
§266. 3 Kb)
§266.35(h)
3. Storage
S266.35(c)
4. Required Notice
§266.35(d)
5. Recordkeeping
§266.35(e)
Standard
Hazardous waste fuel is to
burned in only industrial
furnaces or boilers.
be
A facility burning hazardous
waste fuel must notify EPA
of their activity and obtain an
I.D. number.
Generators that burn and store
the waste within the short
term accumulation period are
subject to $262.34. Existing
storage facilities are subject
to Parts 265, 270 and 124.
New storage facilities are
subject to Parts 264, 270 and
124.
A-one-time written notice to
each marketer certifying that:
1) the burner has notified EPA,
2) has received an EPA I.D.
number, and 3) stating that the
hazardous waste fuel will be
burned in an industrial unit.
Applicable requirements of
264 and 265 and copies of each
certifying notice supplied to
marketers.
40
-------
OSWKK y9'31 .1
Murners:
Hazardous Waste Fuel
266.35(b)
Possible Violations Sect ion
1. Burning hazardous 266.31(b)
waste fuel jj| a
boi ler/f uritjlfci (jhat
does not meer the
regulatory defini-
tion of industrial
provided in the rule,
(see glossary).
2. Failure to notify the
Agency of their waste
fuel burning activity
or obtain I.D. number.
3. Failure to comply with 266.35(c)
storage requirements'/
Parts 265 (Existing
facilities), 264 (New
facilities) and 270.
(Existing is before
May 29, 1986).
Failure to provide the 266.3'5(d)
marketer with the one-
time written required
notice prior to receiv-
ing shipments.
Accepting a hazardous 26!>.76
waste fuel without
proper manifest forms
and fails to report
the shipment.
Supporting Evidence
Sample/information on fuel
in tank and any incoming
fuel shipment. Examine
boiler or furnace to verify
that it does not meet the
regulatory definition of
industrial boiler or
furnace (see glossary).
Check files (and EPA tiles)
to verify absence of noti-
fication or I.D. number.
Clu.'ok for compliance with
storage requirements and
examine for leakage around
tanks. Obtain sample/
analysis of contents. Obtain
photos of any leakage. Check
files for adeguate SI'CC
plan and Contingency Plan.
Check files to verify the
absence of reguird notice
sent. Obtain copy of invoice
for used oil shipments
received prior to notice.
Sample analys i s/informati on
or fuel to determine if it
is a hazardous waste fuel
and examine manifest records
for fuel shipment.
A I
-------
OSWEK 99131.1
Burning hazardous
waste for eneigy
recovery that does
not meet the 5,000
BTU/lb requirement for
fuel. (DoQ£ not apply to
48 FR 11158,
Match 16, 1983
(Note: (3))
Subpart O
Failure to maintain
records for the speci-
fied time period.
266.35(e)
Sample fuel/information
to determine its heat
value
Check files
documents.
and list missincj
42
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OSWEK 9951 .1
Burners: Used Oil Fuel
Requi rements
1. Prohibition
2. Notification
Cite
§266.41(h)
§266.44(b)
3. Required Notice
§266.44(c)
4. Analysis
§266.44(d)
5. Recordkeeping
§266.44(0)
Standard
Off-specification used oil is
to he burned in only industrial
units (.see glossary).
Burning off-spec used oil
requires that the burner notify
EPA of their activity and
obtain an I.I), number.
The burner must provide a one-
time written notice to the
marketing facility certifying
that the burner has notified
EPA and will burn the off-spec
used oil in industrial units.
Generators that burn used oil
claiming it to be specification
are subject to proving the used
oil meets the specs, and burners
that treat used oil to meet the
specs must have analysis or
other information proving it is
spec fue1 .
Copies of invoices, certifying
notices and records of analyses
must be maintained for 3 years.
4 J
-------
OSWER 99S 1.1
Burners; Used Oil Fuel
Possible Violations
1. Burning off-specification used
oil in a non-industrial boiler/
furnace.
Cite
266. 4Kb)
3.
Failure to notify EPA of
their waste-as-fuel burning
activity (if^they burn off-
specification used oil or
blend used oil to meet the
specification as a generator).
Failure to provide the marketer
the required notice certifying
the burner has notified FJPA.
Failure to analyze or provide
other information showing the
used oil the burner blended is
specification. (Applies to any
burner who blends off-specifi-
cation used oil to meet the
specification).
266.44(b)
266.44(c)
266.44H)
5. Failure to maintain the
for the time period.
records
266.44(e)
Supporting Evidence
Fuel information; examine
boiler or furnace to verify
that it does not meet the
regulatory definition of
industrial or facility is
not a manufacturing operation
(see glossary).
Check files (and EPA files)
to verify absence of notice
or 1.1), number.
Check files (and marketer's
files) to verify absence of
certification.
Obtain sample/analysis of
fuel to verify that it does
not meet the specifications,
Document: violation of
requirements for off-spec
used oil fuel.
Check files to verify absence
of required records. List
missing documents. Obtain
copies of inadequate documents
44
-------
Sampling
Equipment preparation for facility inspections will vary
•depending on the facility type and purpose of'ths inspection.
Sampling equipment to be used on the insoection for used oil
storage and transport tanks may include:
o extendable coliwasa: Liquid waste samplers
o weighted bottle samplers
o Bomb samplers
o Pond samplers (Rod and clamp)
Coliwasa samplers can be found in lengths up to 10 feet
which will be sufficient for sampling some underoround storage
tanks. (Underground storage tanks between 8,000 and 12,000
gallons have approximately 8 foot diameter shells and a 2 foot
to 4 foot fill pipe extension to the ground surface).
Weighted bottles and bomb samolers can be used to sample
larger above-ground storage tanks and underground storage tanks
(with man-ways as fill pipe diameters may restrict their use). A
more complete discussion about sampling can be found in Samplers
and Sampling Procedures for Hazardous Waste Streams; EPA-600/2-30-
108. In addition, ASTM-Standard D4057: Standard Practice For
Manual Sampling of Petroleum and Petroleum Products
can be referenced (see appendix E).
A samplfhg plan is a necessary part of the overall inspection
plan. Determine the necessary volume to be sampled, the number
of samples per containment vessel, and arrange for laboratory
support capable of performing analyses using standard operating
procedures. The laboratory conducti^q the analysis should be
45
-------
?S'/ER 9951.1
.consulted to determine the necessary sample size (volume) and
required container. Sampling techniques, including chain of
. custody procedures, should be used that do not jeopardize the
validity of the sampling. A QA/QC review of the sampling protocol
is recommended. Finally, provisions for supplying split samples
to the owner/operator need to be made as part of a sample plan.
Inspecting a processing facility will require thorough record
review and interviews with the owner/operator to determine accurately
the facility processes and operating procedures. The sampling
necessary to establish compliance status may be extensive. For
example, incoming truck loads, storage/processing tanks, outgoing
truck loads and waste streams may all need to be sampled. Therefore,
arrangements for lab. analysis must be established in advanced of
the scheduled inspection.
Containment vessels will vary in size and shape at facilities
storing used oil and hazardous waste fuels. For example, facilities
will use drums, above-ground storage tanks, underground storage
tanks and tank trucks. In addition, waste materials may be
stored in lagoons (surface impoundments). Sampling methods will
necessarily vary depending on the material stored and storage
vessel. The following is a brief discussion of specific situations
~jr
tffe*"
likely to be4Btcountered while sampling for waste fuels.
46
-------
Large_volume (above-ground) tanks will often have faucets
installed or the tanks from which samples can be drawn. Samnling
from, these faucets is acceptable. An important aspect, however,
is co 'nave faucets at different levels on the tank. If a tank
has an adequate circulation system which has been operating for
sufficient time to completely circulate the stored material,
these samples could be taken from one level 'or faucet). Art
inspector must make tank-by-tank judgements as to the adeauacy of
the circulator, system. If a circulation system is relied unon
for mixing the material so as to obtain a homogeneous sample,
the sampling must be done before the material is allowed to
settle. Settling and separation of liquid phases may occur in a
relatively short period of time (e.g. 1 hour or less) in large
tanks. Sufficient circulation time will depend on the tank size,
pump capacity and the material viscosity, and therefore, it is
likely that the owner/operator will need to provide the informati-
indicating required circulation time. Relying on circulation
systems is not necessarily recommended because of the possibility
of incomplete circulation.
A weighted bottle or bomb samoler are other methods for
obtaining samples from tanks or deep lagoons. The tanks should
be sampled atedifferent intervals starting from the top and wor--.:
^
down. A minimum of three (3) levels is recommended using the
ASTM D-405F method. In addition, a Coliwasa may be used to samp:
small tanks, especially underground tanks with small access
ports.
47
-------
OSWER 9951.1
Tan* :ks may need to be sampled and several options
may be app. ;riate. The technique used will depend on the
situation. For example, if a truck is being sampled at a fuel
delivery point, such as a burner, then sampling would best be
conducted during the delivery. Samples can be drawn from the
discharge hose at the beginning, middle and end of the delivery.
This approach provides a representative sample and clearly shews
the sample to be from the fuel that is delivered. Sampling from
the top of the truck is another approach. If the sampling is
done prior to delivery of the fuel, the inspector must be certain
that each compartment of the tank is sampled.1 Furthermore,
the i-nspector must identify which compartment of fuel is delivered
to a facility, and subsequently match the sample to the fuel
delivered.
Obtaining the samples during the delivery is the most assured
means of having the evidence showing a marketing violation if
the fuel is contaminated. This applies to deliveries of waste
oils (hazardous waste) to a recycling facility as well as fuel
shipments to burners. £f samples are obtained prior to a delivery
a facility may turn the truck away or a driver may opt to not
deliver a fuel shipment.
A qualiCJfcassurance procedure using blanks and replicates is
*?*:'
recommended. Blank samples can be prepared using mineral oil of
known quality.
Oil trucks will usually have multiple compartments, (e.g. A
3,500 gallon truck may have 3 compartments of different sizes.)
48
-------
Mineral oil can be used to provide a quality assurance check on
the cleaning of sampling equipment and sample containers.
Mineral oil of known quality should be entered into the samnlinrj
device and then transferred to a clean sample container. In
addition, verification of the sample container cleaning procedures
can be done by sending an empty sample container to the lab
perfroming the analysis. Replicate samples from tanks or trucks
should be taken to demonstrate sample procedure reliability.
This should be done at least once per facility.
Preservation of samples using ice or preservatives is not
necessarily recommended or needed for most used oil/waste fuel
samples. These samples should be treated as hazardous waste
samples and shipped according to DOT standards. Environmental
samples, however, should be preserved for shipment. (See
Appendix F for shipping procedures.)
Finally, sample equipment cleaning may be necessary on site
if more than one containing vessel is to be sampled. A procedure
recommended for cleaning samplers contaminated with used oil is
the use of unleaded gasoline and a soap wash. The following
steps are 1:2commended: (1) rinse the equipment with the unleaded
gasoline; (2X.wash with soap and water; (3) rinse with clean
>• "w'•
water folloMfljfcjby; (4) an acetone rinse and air drying.
49
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Analytical Methods
Analytical methods are recommended in the preamble (30 FR
49139, N'ovember 29, 1935) and shown in Table I of this document.
Although these are the procedure recommended to the regulated
community, they are not necessarily the methods the Agency will
use for sample analysis. A factor that must be considered when
evaluating a facility's analytical results is the precision and
accuracy of the recommended methods. There are variations of
these methods, and therefore, it should be specified by the facility
as to which is used.
The analytical program employed by the Regions can vary in
approach. However, use of any analytical methods for sample
analysis should be preceded by OA/QC protocols evaluating the
method performance. Additional methods reviewed by the Office of
Solid Waste will be presented in a report.
Screening methods may prove to be valuable in the field and
laboratory. If a reliable field test method is developed for
total halogen (TX), it may be useful for conducting more efficient
inpsections involving sampling (i.e., it may help focus the
sampling to those materials most highly contaminated). Another
approach to screening samples can be applied in the laboratory.
*w-
Samples coul^jjpr screened <£or TX and subsequent analysis could be
done for specific compounds. The approach selected will be
dependent on the resources available for sample/analysis programs.
50
-------
OSWER 9951.1
Identifying a fuel oil to be a used oil may be an essential
aspect of the analytical results should a facility deny the
presence of used oil or other wastes. In addition to the speci-
fications for used oil, several indicator oarameters may be
selected as criterion for determining if a fuel oil is contaminated.
As a general rule, chlorinated organic compounds will not be
found in virgin oils. Chlorinated solvents are not added to
fuels or lubricating oils during refinina. These compounds (e.g.
F001 and F002 wastes) even if present at extremely low levels
(less than 100 ppm) would be a definite indication that the fuel
is contaminated and may be a used oil mixture if not a hazardous
waste mixturee. A group of chlorinated organic compounds, parafins,
although not hazardous wastes would indicate that used oil is
present in the fuel. These parafin compounds are additives to
certain lube oils.
Metals are another mean of establishing the presence of used
oil or hazardous waste blends in fuels. Generally, if several of
the four metals (lead, arsenic, cadmium and chromium) established
as the standards for specification oil are exceeded by any measureable
amount, then it is reasonable to assume the fuel to be used oil.
In cases wher» only one or two of the specs for metals are exceeded,
' -I*
^^to&-
then the pr0fl|pce of other metals, such as zinc and barium,
would provide substantiating data that used oil is present.
(Appendix G provides a list of lubricating oil additives, and
tables of contaminant concentrations in used oil samples).
51
-------
OSWER 9951.1
Analysis to support the presumption of nixing will be an
essential element to any -enforcement .action. As stated in the
regulations, used oil containing a total halogen (TX) level in
excess of 1000 ppm is presumed to have been mixed with hazardous
waste. Note, it is not necessary that the total organic halogen .
level be over 1000 ppm to trigger the presumption. It is necessary-,
however, that sample analysis go beyond the identification of
TX. The analysis should proceed to the identification of specific
chlorinated organic compounds. If listed hazardous waste in the
form of chlorinated organics (e.g., F001 and F002 wastes) are
found at significant levels, the presumption that hazardous
waste is present is substantiated. Significant levels in this
case would be in excess of 100 ppm for any individual compound.
Additional rebuttals may be presented on the basis of specific
exemptions. However, the analytical data should be available to
support the initial conclusion by the Agency that a hazardous
waste is present.
52
-------
CS:/ER 9951.1
Glossary
Hazardous Waste Fuel;
Any fuel that has been mixed with a listed hazardous wasta
and used as a fuel or distributed as a fuel is considered a
hazardous waste fuel (Section 3004(g)). In addition, used oil
that continues to exhibit a characteristic, as defined by Part
251, after being mixed with a characteristic hazardous waste is
a hazardous waste fuel. Used oil with total halogen levels
exceeding 1,000 pom is presumed to have been mixed with listed
hazardous waste, and therefore, is regulated as a hazardous
waste fuel. (Used oil with flash point below 100°F is regulated
as off-specification used oil.) Exception: used oil or other
virgin fuel mixed with a small guantity generator (less than one
hundred kilograms per month) hazardous waste is not regulated as
hazardous waste fuel, regardless- of the total halogen level, but as
a used oil. (Mote: Future rules may change this exception). In
addition, a minimum 5,000 to 8,000 BTU per pound (3TU/lb) heat
value must be met for hazardous waste to be considered a fuel,
otherwise it constitutes "sham recycling." (48 Federal Register
11158 (n.3), March 16, 1983)
2. Industrial Burners (Boilers and Furnaces)
EPA def^fte the term "industrial boiler" as any boiler that
produces electric power, steam or heated or cooled air, or other
gases or fluids for use in a manufacturing process, or any boiler
located on the site of a manufacturing facility. Further, EPA
has defined "boiler" as an enclosed device using controlled flame
, 53
-------
OSWER 9951.1 . .
combustion and having specific characteristics including: (1) the
combustion chamber and primary energy recovery must be of intearal
design; (e.g., waste heat recovery boilers attached to incinerators
are not boilers); (2) thermal energy recovery efficiency must be
at least 60% and (3) at least 75% of recovered energy must be
"exported" (i.e., not used for internal uses like preheating of
combustion air or fuel, or driving combustion air fans or feedwater
pumps). See 50 £R at 661 (January 4, 1985).
"Industrial furnace" means any of the following enclosed
devices that are integral components of manufacturing processes
and that use controlled flame devices to accomplish recovery of
materials or energy:
( 1) Cement kilns
(2) Lime kilns
(3) Agaregate kilns
(4) Phospate kilns
(5 ) Coke ovens
(6) Blast furnaces
(7) Smelting, melting, and refining furnaces (includina
pyrometallurgical dev-ices such as cupolas, reverberator
furnaces, sintering machine, roasters, and foundry
furnaces)
( 8J Titanium dioxide chloride process of oxidation reactors
(9) Pulping liquor-recovery furnaces
(10) Methane reforming furnaces
(11) Combustion devices used in the recovery of sulfur values
from spent sulfuric acid
(12) Such other devices as the Administrator may, after notice
and Comment, add to this list on the basis of one or more
of Ujjfe. following factors:
(a) The design and use of the device primarily to accomplish
recovery of material products;
(b) The use of the device to burn or reduce raw materials
to make a material product;
54
-------
OSWER 9951.1
(c) The use of the device to burn or reduce secondary
materials as effective substitutes for raw materials,
in processes using raw materials as principal feed-
stocks ;
(d) The use of the device to burn or reduce secondary
materials as ingredients in an industrial process to
make a material product;
(e) The use of the device in common industrial practice to
produce a material product; and
(f) Other factors, as appropriate.
(Note: Aggregate kilns include asphalt kilns).
3. Invoice:
A record of shipments delivered or received for off-specifi-
cation used oil fuel. The following information is to be included
on each invoice: 1) invoice number, 2) individual's U.S. EPA ID
no., 3) receiving facility EPA ID no., 4) name and address of
shipping facility 5) quantity of fuel shipped, 6) date(s) of
delivery, and 7) the following statement, "This used oil is subject
to EPA regulation under 40 CFR Part 266." (see 5266.43)
4. Manifest;
A standard transportation form required for the transportation
of hazardous waste as regulated under RCRA, i.e., the Uniform
Hazardous Waste Manifest (EPA Form 3700-22/22A). (see definition
in §260. 10)
f**"
5. Off-speq^ftcation Fuel;
Used oil being recycled for energy recovery that has not
been mixed with a hazardous waste, but does exceed a specifi-
55
-------
OSWER 9951.1
cation level established for metals, total halogens or flash
point (S266.40(e)).
To clarify footnote (a), generally, used oil mixed with
hazardous waste is considered a hazardous waste fuel, and therefore,
the specifications are not relevant. However, there are exceptions,
one of which is small quantity generator hazardous waste mixed
with used oil. This mixture would be subject to the specifications
under Subpart E and not regulated as a hazardous waste fuel.
USED OIL EXCEEDING ANY SPECIFICATION LEVEL
IS SUBJECT TO THIS SUBPART WHEN BURNED
FOR ENERGY RECOVERY a/
Constituent/Property
Arsenic
Cadmium
Chromium
Lead
Flash Point
Total Halogen
Allowable Level
5 ppm maximum
2 ppm maximum
10 ppm maximum
100 ppm maximum
100° F minimum
4000 ppm maximum b/
a/ The specification does not apply to used oil fuel mixed with
a hazardous waste other than small quantity generator hazardous
waste.
b/ Used oil^CBitaining more than 1000 ppm total halogens is
presumed to be a hazardous waste under the rebuttable presump-
tion provided under $266.40(c). Such used oil is subject to
Subpart D of this part rather than this subpart when burned
for energy recovery unless the presumption of mixing can be
successfully rebutted.
-------
OSWER 9951.1
6. Rebuttable Presumption;
Used oil which contains in exces of 1000 ppm total halogens
is presumed, subject to rebuttal, to have been, nixed with a
halogenated hazardous waste. Such used oil is regulated as a
hazardous waste under the "mixture rule" of 40 CFR §261.3, which
provides that a mixture of hazardous waste and other material is
a hazardous waste. The presumption of mixing may be rebutted,
however, if .the owner can show that the used oil has not, in
fact, been mixed with hazardous waste.
7. Required Notice;
A one-time written notice certifying that an individual
(company) has notified EPA or authorized state of their hazardous
waste fuel or used oil management practices and will burn off-
specification used oil or hazardous waste fuel only in an industrial
boiler or furnace as defined in S266.31(b). The notice must be
sent by the owner/operator to each facility with which he has'
transactions involving used oil/waste fuels and a copy of the
notice must be retained. This requirement applies to both the
shipping and receiving facilities.
8. Specification Fuel: (Spec Fuel)
A used oil is a spec fuel if it does not exceed the levels
^SL.
for metals afllfchalogens or fall below the flash point establishe i
.^r!^'
in $266.40(e), and it has not been mixed with hazardous waste.
9. Used Oil:
Any oil refined from crude oil, used, and, as a result con-
taminated with physical and chemical impurities. (See RCRA
57
-------
OSWER 9951.1
section 1004). Included are the following: spent automotive
Lubricants and fluids (engine oils, transmission fluid, brake
flui-.-i and off-road engine oil); spent industrial oils, (compressor,
turbine and bearing oils) hydraulic oils, metal working oils,
refrigerator oils, railroad drainings; and spent industrial process
oils. (50 FR 49174, Nov. 29, 1985).
58
-------
9951.1
Appendix A
Used Oil Processina
-------
9951.1
INDUSTRY PRACTICES FOR USED OIL PROCESSING FOR FUELS AND LUBE STOCK
There are a number of processes applied to used oil for use as a fuel or
as re-refined lube stock. These processes include:
Settling ° Acid clay
Filtration ° Vacuum distillation
Dehydration (heat addition) ° Wiped film distillation
De-emulsion ° Hydrofinishing
Centrifugation ° Clay contacting
Blending
In addition, used oil is sometimes collected and sold or used as fuel without
any treatment. In the no treatment case, a truck typically collects oil from
one or more sources and delivers it directly to a fuel user.
Most used oil is subject to minor processing before being sold as a
fuel. Settling and filtration are nearly universally used processes; they
are designed to remove bottom sediment and water (BS&U) through simple physi-
cal separation. Settling is generally accomplished by pumping the oil into a
tank and allowing gravity settling to occur, followed by removing the oil
layer for use. The water layer may sometimes be added to other batches of
oil that are low in water, but usually it is disposed of as a wastewater. In
some cases oil is stored and settled in drums, surface impoundments or col-
lection ba: is; however tanks are most commonly used.
In addition to settling, filtration is almost always used to reduce
sediment and other solids from oil. Often the oil collection trucks and-the
waste oil tanks have filters in the lines so that the oil 1s filtered as it
is transferal from tank to truck or vice versa. The solids collected on the
filters arMBpoved periodically and disposed of as a solid waste. Process-
ing equlpmTfW In-line filtration and gravity settling consists of storage
tanks, pumps and hoses, (plus drums and surface impoundments, where appli-
cable).
Heat 1s used to enhance the separation of oil from water mixed with
light end fuels and gasoline, and to separate light end fuels and gasoline
1
-------
S5WER 9931.1
(see Figure 1). This process, dehydration, is accomplished by heating the
oil to decrease viscosity and improve gravity settling; this is usually done
in a settling tank. (Waste oil may be used as the fuel to supply the heat.)
Steam condensate is formed in the cooling lines and becomes part of the
wastewater stream. The wastewater from this process will likely contain
volatile organfcs, such as TCE, 1,1,1-trichloroethane and trace fuel products.
Settling, filtration and heating are primarily used to reduce water,
solids and some of the light hydrocarbons which affect the oil. Heavy metals,
organics and other potentially hazardous constituents which are solubilized
in the oil are not significantly affected by these minor treatment processes.
Analytical data indicates that only re-refining reduces hazardous constitu-
ents in used oil.
Used oil can form emulsions as a result of fuel additives and other
materials from automotive or industrial uses. Some hydraulic fluids, lubri-
cants and coolants are formulated as oil-water emulsions containing mostly
water (60 to 952) and lesser amounts of oil. Agitators are used to mix
emulsion-breaking chemicals in waste oil. Settling follows the agitation,
and the resulting wastewater layer is separated from the oil layer. De-
emulsion by agitation and settling is performed in tanks or surface impound-
ments; tanks are generally above-ground and may be open-topped.
Centrifuges are used by some used oil processors to remove fine solids
from oil. Filter screens are also used for the same purpose. Centrifuge or
filter screen solids are usually disposed of as a solid waste at sanitary
landfills, however, they may be sent to hazardous waste landfills, incin-
erated or sold to asphalt plants as asphalt extenders or fuel. The waste-
water is most commonly treated at private treatment or recovery facilities;
alternatively it may be stored in surface impoundments or evaporation ponds,
or may be discharged to the sanitary sewers.
Blending Is done by processors to mix treated oil with untreated oil,
virgin fuel|g£ls or solven^ (usually non-chlorinated) to achieve desired ena
products. ITending Improves oil quality by diluting the concentration of
undesirable contaminants. Most typically, blending refers to mixing proc-
essed used oil with virgin fuels (No. 3, 4, 5 and 6 and diesel fuel).
Blended fuel oil products typically contain 5 to 20 percent used oil; they
are usually sold directly to end-user's by virgin fuel oil dealers who do t"e
-------
OSWKK 09'i |.l '
Figure 1
WASTE OH.
SIEVE SHAKER
{REMOVES RAOS, LEAVES
AND MISCELUUBMIft SOLIDS
SOUDS TO
NOTE: PRESSURE FILTER OR
VACUUM FILTER CAN BE USED
IN LIEU OF CENTRIFUGE
HEAT
CHEMICALS FOR
pH. EMULSIONS. ETC.
TO DISPOSAL
(
WATER TO
TREATMENT
HEAT
TO DISTILLATION
-*. TO CONSUMER
WASTE OIL
RECEIVING TANK
HEATING/MIX
TANK
CENTRIFUGE
(CAN BE HORIZONTAL
OR VERTICAL)
PROCESSED OIL
WATER SEPARATOR
FUEL PROCESSING
HEATING, TREATING, AND CENTRIFUGING
-------
blending in their tanks. In addition to mixing processed oil with virgin
fuel oil, treated oil may be mixed with other used oil. Used oil that is
high in water may be blended with other used oil to achuve a blend with an
acceptable 8S4W level. Some processed oils are blended with solvents to
decrease oil viscosity or as a means of solvent disposal.
Blending can be done according to various end product specifications.
Some blenders mix a given ratio of processed used oil with virgin fuel oil.
Other specifications for blending include product viscosity, heat content,
percent solids, or percent moisture. Because these specifications require
that the blender conduct some analyses of the oil, most blenders have desig-
nated receiving tanks for storage of used oil. After analysis to determine
blending ratios necessary, the used oil is usually pumped and metered into a
blending tank where it is mixed with a measured volume of virgin fuel oil,
other used oil, etc. The oil is blended using mechanical mixers, aeration or
in-line mixing. The blended oil is usually pumped to a storage tank or to a
truck for delivery to a user.
Figure 2 is a schematic showing used oil processes for fuel production,
the residues generated from them, and their usual disposal/treatment alter-
natives.
The remaining processes, acid clay, vacuum distillation, wiped film
distillation, hydrofinishing and clay contacting, are all re-refining tech-
niques that change the quality of used oil from a contaminated waste to a
useful product with reduced levels of contaminants. Re-refining is practiced
by only a small number of facilities (about 9 facilities 1n 1984). Re-re-
finers are usually larger than used oil processors; however, due to their
small number, they collectively handle less than 15 percent of used oil which
is collected. Typical re-refiners process 8 to 10 million gallons of used
oil per year. Larger ones may process up to 20 million gallons of used oil
annually. -^
The ad^flay process was practiced in 1983 by only 2 or 3 facilities
which each handled 2 to 4 million gallons per year. The process basically
is conducted In three parts: a dehydration step, the acid treatment, and the
2
clay treatment. In the dehydration step, filtered oil is heated in a tank
to remove water. The dehydrated oil js then pumped to an acid treating unit
where it is agitated with air and mixed with acid for 24 to 48 hours. An
-------
Appendix B (1-3)
-------
OS'.VER 99 5
APPENDIX B-1
Effective Dates
Requirement Date
Prohibitions December 9, 1985
Used Oil.Specification
(except lead specification)
Rebuttable Presumption
Analysis 5 Recordkeeping
for Specifications
Notification January 29, 1986
Other Recordkeepina March 31, 1936
(Manifest, Invoice,
Certification Notice)
Part A Permit Applications May 29, 1986
(Hazardous Waste Fuel
Storage)
Storage Controls
Lead Specification
-------
OSWER 9951.1
Appendix B-2
Invoice System:
1. Invoice Number
2. Sender's EPA Identification Number
1. Receiver's EPA Ident if. icat ion Mumbar
4. Barnes and Addresses of Shipping and Receiving Facilities
5. Duantity of off-specification used oil to be delivered.
6. Oate(s) of shipment or delivery.
7. Statement: "This used oil is subject to EPA Regulation
under 40 CFR Part 266."
-------
OSWER 9951.1
Appendix B-3
Reauired Notice:
1. One-time written notice.
2. Certifies that the marketer or burner has ixotified EPA of the
location and general description of the hazardous waste fuel
and used oil activity.
3. Burners must state that hazardous waste fuel and off-specifi-
cation used oil fuel will be burned in industrial boilers or
furnaces, only.
4. Notice must be provided before a marketer may ship off-speci-
fication used oil or hazardous waste fuel to another marketer
or burner.
-------
OSWE?. 9951.1
Appendix C
Checklist
-------
U..WKK
.]
NOTE: * DENOTES MOST COMMON METHODS OF RESIDUE MANAGEMENT.
SOURCE: REFERENCE I.
Figure 2. Processing residue generation and management.
-------
OSWER 9951 .1
acid sludge containing oxidized contaminants and ash is removed from the
bottom of the reactor and disposed, most often at a hazardous waste landfill.
The treated oil is then transferred to a clay treatment tank (a 5,000 to
10,000 gallon tank) where it is stripped with steam to remove light fuel
fractions and subsequently slurried with clay (usually activated clay and
diatomaceous earth) to remove inorganic contaminants (metals, color bodies
and collida'l carbon). The hot oil and clay is then filtered. The clarified
oil is mixed with additives; the resulting blended oil is the lube oil pro-
duct. The spent clay is usually landfilled.
Figure 3 shows the acid/clay re-refiner residue generation and manage-
laj
ment. An acid clay re-refiner typically generates the following amounts of
residues annually:
In-line filtered residue 200 to 2,000 pounds
Wastewater 100,000 to 1,000,000 gallons
Acid sludge 250,000 to 750,000 gallons
Spent clay 300 to 500 tons
Most re-refiners use vacuum distillation technologies to produce lube
oil stocks from used oil. Used oil is filtered and heated in a direct heater.
It is then sent to a flash tower where oil/water overhead is condensed; the
light fuel is used in the plant and the wastewater is treated. Caustic and
light oil (naptha) are added to the flash tower bottoms to break oil-water
emulsions and precipitate solids. The solids are removed as a sludge from a
centrifuge. This is considered pretreatment. The pretreated centrifuged oil
is pumped to a vacuum distillation tower where it is heated under a vacuum
(700°F and 27" mercury). Three streams are produced. The overhead light
fuel (naptha) 1s condensed and reused in the plant. The ash-containing
bottoms are often used by asphalt plants. The middle stream is the lube oil
stock; it may be finished using a clay treatment (clay slurrying and filtra-
tion), folljiift by blending, with appropriate additives.
Figure£pep1cts vacuum distillation re-refiner residue generation and
management. A typical vacuum distillation generated the following amounts
of residues annually:
In-line filtered residue 500 to 5,000 pounds
Wastewater 250,000 to 2,000,000 gallons
Spent clay ' 500 to 2,000 tons
-------
OSWKK
WASTE OH.
GENERATOR
£
IN-LINE
FILTER
COLLECTION
TRUCK
IN-LINE
FILIER
MI WITH
MUNICIPAL
WASTE
DEHYDRATION
UNIT
ACIO
TREATMENT
CLAT
CONNECTING
LUBE OH
BLENDING
* + * *
•RICK/ffAVMa
MATERIAL
SECURE
LANDFILL*
ACIO
RECOVERY
•FUEL
* * t
LANDFILL*
BURN FOR
FOR RECOVERY
REGENERATION
NOTE: * DENOTES MOST COMMON METHODS OF RESIDUE MANAGEMENT.
SOURCE: REFERENCE 1.
Figure 3. Acid/clay re-refiner residue generation and management.
-------
U.'.WI.K
WASTE OIL
GENERATOR
^
IN LINE
FILTER
COLLECTION
TRUCK
IN-LINE
FILTER.
HEATED
SETTLING
00
( FILTER A
V RESIDUE I
MIX WITH
MUNICIPAL
WASTE
SKIMMED
OIL
IMPOUNDMENT.
EVAPORATION
POND9
SANITARY
SEWER*
STORM SEWER
NOTE: * DENOTES MOST COMMON METHODS OF RESIDUE MANAGEMENT
SOURCE: REFERENCE 1.
Figure 4. Vacuum distillation re-refiner residue generation and management
-------
listing wastes from the manufacture of UDMH as hazardous under
RCRA,'7 since EPA believed that this data provided strong evidence
that UDMH is a carcinogen. Uniroyal responded to the August 17,
1989 Notice of Data Availability with the following contentions
that the data did not support a determination that UDMH was a
probable human carcinogen. The specific challenges to the
significance of these data for a carcinogenicity determination
are given below.
a. Uniroyal claimed that the biological significance of
the interim results of the UDMH and Daminozide study are
questionable. For example, while positive tumorigenic results
were seen in mice, no significant increases in tumor incidences
were detected in any of the exposed groups of rats.
Response; The lack of detectable effects in rats cannot be
construed as evidence for noncarcinogenicity. Only an extremely
potent carcinogen would be expected to induce an increase in
tumor incidence as early as 12 months from the start of exposure.
In fact, the positive results seen in mice as early as 8 months,
suggest that UDMH is not only a carcinogen, but a rather potent
one. Furthermore, it is generally recognized that species may
differ in sensitivity to an applied dose, so the interim results
with rats is not inconsistent with this expectation.
I754 FR 33942.
-------
gain or loss of specific enzyme systems in the hepatocytes.
Since the cells are rapidly dividing, one enzymatically altered
cell will reproduce to form an "island" of similar cells. These
islands can be made visible by differential staining techniques.
The assay is regarded as a test for probable carcinogenicity
since the enzymatic changes are considered by many investigators
to be early steps in the progression of cellular changes leading
to cancer.
The tumors, however, occur in blood vessels, a different
type of tissue than located in the liver. Thus, the lack of any
increase or severity of the liver islands does not negate the
carcinogenicity determination.
c. Uniroyal argued that since positive results were seen
in mice only at 40 and 80 ppm, dosages that Uniroyal claims are
clearly in excess of the maximum tolerated dose (MTD), any
conclusions on the carcinogenicity of UDMH based on results from
tests which exceeded the MTD are not valid.
Response; According to established Guidelines18 using body
weight gains, survival, etc., EPA believes that the MTD was not
exceeded. Mortality that did occur during the first 12 months of
exposure was considered by the EPA auditors19 to more likely be
the result of cancer rather than liver necrosis. Since tumor
increases were detected in intermediate dosed males as well as in
females, in which the pathological effects and other toxic signs
18U.S. EPA (September 24, 1986), ibid.
19U.S. EPA, OPP (April 22, 1985), ibid.
10
-------
were minimal, the results are not considered to be invalidated by
the debatable overdosage.
Even if the MTD was exceeded, the data can be used in
assessing carcinogenicity according to EPA's risk assessment
Guidelines, if the results are carefully reviewed to ensure that
responses are not due to factors operating only at levels above
MTD.20 These include effects such as metabolic activation at
high concentrations and hormonal changes. There is little
information to indicate that UDMH requires this type of
activation, however, which would call into question the
possibility that the observed effects were due to an exceedance
of the MTD. In addition, there is also no data to indicate that
important hormonal.changes are taking place, another effect that
could be caused if the MTD were exceeded.
The pathological changes in the liver would be of serious
concern in evaluating whether the MTD had been exceeded if the
liver itself was the primary target organ for the carcinogenic
effects of UDMH. The possible genetic alterations with increased
cell turnover rates resulting from the pathological changes could
lead to tumor induction in some cases. UDMH, however induces
tumors in blood vessels and not in the liver itself. As a
results, the changes in the liver do not confound the
observations of carcinogenic effects in other organs, the blood
vessels.
20U.S. EPA (September 24, 1986), ibid.. pp. 1-5.
11
-------
The pathological changes in the liver would be of serious
concern in evaluating whether the MTD had been exceeded if the
liver itself was the primary target organ for the carcinogenic
effects of UDMH. The possible genetic alterations with increased
cell turnover rates resulting from the pathological changes could
lead to tumor induction in some cases. UDMH, however induces
tumors in blood vessels and not in the liver itself. As a
results, the changes in the liver do not confound the
observations of carcinogenic effects in other organs, the blood
vessels.
Thus, EPA does not believe that the MTD was exceeded in the
recent Uniroyal studies. Secondly, even if the MTD has been
exceeded, EPA's careful review of the data has ascertained that
the carcinogenic effects were independent of any physiological
changes which could have been caused by an exceedance of the MTD.
The results, therefore, still may be used to determine that UDMH
is a carcinogen.
d. Uniroyal claimed that the carcinogenic effects were
accompanied by a variety of hematological, liver enzyme and liver
pathology changes that may well have been responsible for the
tumor induction. Thus, the commenter contended that the tumors
should not be considered to be the result of a carcinogenic
effect of UDMH.
Response; The hematological, liver enzyme, and liver
pathology changes are considered by EPA to be a result of tumor
growth and are thus not responsible for their induction. In
12
-------
other words, these changes are considered to be the result of the
carcinogenic effects of UDMH, and not some side effect unrelated
to carcinogenesis. In addition, it should be noted that tumors
were induced in females in which alterations of liver enzyme
activity and hematological parameters were minimal. Finally,
increased tumor incidences were also seen in the lungs, an organ
showing few indications of pathological changes. Thus, the
Agency does not agree that the observation of hematological and
liver changes negates a conclusion that UDMH should be considered
a causative agent for carcinogenesis.
e. In general, Uniroyal contended that the weight-of-
evidence from the interim results of the studies on UDMH
carcinogenicity did not support a determination that UDMH should
be classified as a category "B2" carcinogen, a "probable human
carcinogen."
Given that significant increases in tumor incidences were
seen at more than one site, in both sexes of mice, and to occur
very early, and because the responses occurred in the lungs even
at lower, relatively non-toxic doses, the newer, interim data is
considered by the Agency to be consistent with the earlier data
regarding the carcinogenicity of UDMH.
According to EPA's Guidelines for cancer risk assessment, a
chemical is classified into category B2 when there is sufficient
evidence for carcinogenicity in animals, but insufficient data in
humans. Sufficient evidence for carcinogenicity in animals
occurs when there is an increased incidence of malignant or
13
-------
combined benign and malignant tumors (a) in multiple strains or
species (b) in multiple experiments (e.g., with different dose
levels) or (c) to an unusual degree in a single experiment. The
interim results of the studies satisfy both categories "a" and
"c" in that significant tumor increases occurred in both mice and
hamsters and the response occurred to an unusual degree, e.g., 84
percent incidence of hemangiosarcomas in male mice. Thus, since
human data is inadequate, while animal data is sufficient, UDMH
is still considered to fit the classification weight-of-evidence
category B2.
f. Uniroyal claimed that the interim data were also
inadequate to establish a quantitative, or dose-response, risk
estimate for UDMH.
Response; The Agency need not develop quantitative weight-
of-evidence for a potential carcinogen as a necessary basis for a
determination that a toxicant of concern or wastes containing
that toxicant should be regulated as hazardous under RCRA.
Available studies on UDMH do indicate that it is a potent
carcinogen. The final studies on UDMH carcinogenicity to be
submitted to EPA in the future are not likely to alter this
evaluation.
g. Uniroyal also claimed that the results from the interim
studies being conducted by Uniroyal demonstrated that UDMH was
not mutagenic.
Response; A total of 5 mutagenicity studies were submitted
to EPA as part of the interim results on UDMH oncogenicity during
14
-------
1989. Three were considered to be negative and acceptable, the
Ames Salmonella test, unscheduled DNA synthesis, primary rat
hepatocyte and CHO/aberration. The use of an unusual solvent
0.25 N HC1, however, limits the interpretation somewhat. Two
CHO/hprt gene mutation assays were also submitted, one using the
0.25 N solvent. In the second, an attempt was made to buffer the
solution. In these latter two studies there were enough
instances of elevated frequencies to suggest that there may be
mutagenic activity. Taken as a whole, therefore, the results
must be considered to be equivocal, rather than negative. They
also do not discount the validity of the earlier tests that were
positive since conditions varied somewhat with each test.
(**Will expand this section later.**)
In summary, after carefully evaluating the comments, the
Agency believes that the available evidence supports a
determination that UDMH is carcinogenic.
15
-------
Wiped-film distillation, hydrofinishing and clay contacting are varia-
tions of the acid clay and vacuum distillation re-refining technologies just
discussed. The wiped-film distillation occurs in a distillation column and
removes water and the light oil fraction from the used oil. Hydrofinishing
involves reaction of the lube oil distillate the hydrogen over a HCl-re-
sistant catalyst to remove nitrogen, oxygen, chlorine and some sulfur-bearing
organic compounds. The hydrofinishing process produces saturated hydro-
carbons and HC1, water, ammonia and hydrogen sulfide. Clay contacting re-
moves metals and other inorganics (see previous discussion).
-------
OSWER 9951.1
RCRA Checklist for Generators Recycling Wastes To 3e Burned
for Energy Recovery
Name of Facility:
Address:
EPA r.D. Number:
Facility Inspection Representative
Title:
Telephone Number:
These are questions pertaining to owners and operators who recycle
wastes to be burned for energy recovery.
1. Does the facility generate any hazardous wastes? yes no
2. Has the facility identified all hazardous wastes
generated on site in accordance with §262.11? yes no
3. Does the facility classify as a generator regulated
under RCRA generator regulations? yes no
If yes, then refer to the appropriate checklist
for generators: Small Quantity or Generators.
4. Does the owner/operator market waste as fuel
directly^to burners? yes no
If yea, Upon refer to the marketer checklist.
5. Does the facility ship hazardous waste off-site? . yes no
If yes, review the facility records for the
required manifests for shipments. (§262.20)
*
6. Does the facility recycle used oil, i.e., ship
used oil off-site? (specify where if possible) yes no
-------
OS WE a 9951.1
7. Does the facility burn its waste as fuel for
. ' energy recovery? yes no
If yes, then refer to the burner checklist.
Inspector's Name:
Title:
Agency:
Office Location:
Date of Inspection:
Comments:
-------
RCRA Checklist £or Inspection of Waste Fuel Marketers/Processors
Name of Facility:
Address:
EPA Waste Fuel I.D. Number:
Facility Inspection Representative:
Title:
Telephone:
Site Characterization:
1. Does the facility accept hazardous waste?
2. Does the facility blend hazardous waste with
oil to be marketed as fuel?
3. Does the facility accept hazardous waste fuel/
i'.e., used oil previously blended with hazard-
ous waste?
4. Check the following general operatina practices:
yes
ves
yes
no
no
.no
Storage
Drum
Above-ground tank(s)
Underground tank(s)
Other
Tank siz**
Descriptions and
Observations:
Treatment
Settling
Heat addition
In-Line Filtering
Certrifugation
Screen Filtration
Dehydration
Emulsion Breaking
Blending
Disposa1
Landfill
Land Treatment
Surface .
Impoundment
Other
-------
OSWER 995 L.I
5. Does the facility have Interim Status or a
permit (Section 3005)? yes no
Specify: .
6. Does the facility generate hazardous waste? yes no
7. Does the facility accept hazardous waste? yes no
specify waste and generator type.
(Request manifests for review)
Small Quantity Generators
( <100kg/m or 100 £1000 kg/m)
Large Quantity Generators
Specify waste types:
8. Does the facility accept only used oil? yes no
9. Specify other material recycled as fuel.
10. Has the facility notifed the Agency of their waste
fuel activity? (§266.34(b)) ' yes no
If no, explain: '
11. Does the facility have manifests for all shipments
of hazardous waste and blended hazardous waste
fuel (received or sent)? (§265.70) yes no
12. Does theacility have a copy of the required
notice £•• burners or marketers to whom waste
fuel is W&keted? ($266.34(e) or §266. 43(b) ( 5) ) yes no
13. Does the facility have invoice information for
shipments of used oil claimed to be specifica-
tion used oil fuel? (§266. 43(b) (6) yes no
-------
OSWER 9951.1
14. Does the above invoice information for
specification used oil fuel have a cross-
reference to analysis or other information? yes no
15. Does the facility analyze for metals and
halogens? yes no
Specify methods:
16. Does the facility have records of analysis
or other information used to claim used
oil meets the specification? yes no
17. Does the facility have the records required
under §266.34(f) or §266.43(b)(6)? yes no
Comments:
Mote: If a facility markets hazardous waste fuel, the facility.
is subject to storage requirements of Parts 262, 264 or 265
and 270, Subparts A through L. Therefore, the RCRA checklist
for inspection of JTSD Facilities may be useful.
Inspector's Name:"
Title:
Agency: ':
* -f ^SMM..
fSCl '
office Locatibat
Date of Inspection:
-------
OSWER 9951 .1
RCRA Checklist for Burners of Used Oil Fuel
and Hazardous Waste Fuel
Name of Facility:
Address:
EPA Waste Fuel I.D. Number:
Facility Inspection Representative:
Title:
Telephone:
The following questions pertain to facilities regulated under
Part 266 who are burning waste fuel for energy recovery. These
do not necessarily apply to incineration under Subppart 0 of part
265.
1.
2.
3.
4.
5.
Does the facility burn used oil fuel?
Specify: off-specification specification
Does the facility burn hazardous waste fuel?
Does the facility's burning unit(s) classify as
industrial boiler(s) or industrial furnace(s)?
Has the owner/operator notified EPA of their
waste fuel activity? (§266.35(b) or §266.44(b))
Was the flwility existing before May 29, 1986?
yes
yes
yes
yes
yes
no
no
no
no
no
6. Does th^^Scility have records of the required
notices sent to the fuel suppliers (marketers)
for hazardous waste fuel or off-specification
used oil? ($266.35(d) or §266.44(c)) yes no
7. Does the facility have Interim Status or a yes no
permit (§3005)?
Note: Storage requirements under Subparts A through L, Parts 262,
264 or 265 and 270 apply to these facilities as of May 29,
1986. Therefore, refer to the RCRA Checklist for inspecti-:-
of TSD Facilities.
-------
OSWER 9951.1
Comments:
Inspector's Name:
Title:
Agency:
Office Location:
Date of Inspection;
-------
Appendix D
Samplinn Methods
ASTM D 4057
-------
9 5 L. 1
Designation: 04057-a 1"
MPMS (Ch*pt«f 0.1)
AMEB.CAM SOClETv «OB 'ES*'NG *NO MATERIALS
<9<9 Out Si "Mict'O"'! pi '"03
n*0"iitO 'ram mt Annual 8oo« 01 ASTM Sunol'OJ Cooyrigm ASTU
it 101 i-stfO noti *"' 100*4' >" mt ^tit tditton
Standard Practice for
MANUAL SAMPLING OF PETROLEUM AND PETROLEUM
PRODUCTS'
Thii iuadard u uiiwd uadcr th< Aud daiguuoa O 4057: UM auatatr ummduiciy foUoviot UM dcugoiuo* urti-'vf* ib*
yur of onainil adopuea or. in UM cu» of rcvuio*. i4« y««f of Lut rrruwa. A auabtr ui parcntbtMi ladwiMi UM j^w o«" Uat
(ctppravti. A tupcnenpi tpuJos («) iadiaui ta iditonal cbioft iue* (be UM revuioo or rtapproval
" Non— An editonaJ correction *u mad* in Ftf. 6 in November 1984.
'' Norr^An ediiond cornelian •*> made in 1.6.4 in November 191).
1. Scopt
1.1 This practice coven procedures for ob>
uioiag represenuuve samples of stocks or ship-
menu of uniform petroleum products, except
electrical insulating oils and fluid power hy-
draulic fluids. This method also does not cover
butane, propane, gas liquids at or above 26 psi
(179 kPa) Reid vapor pressuretRvp), and other
petroleum products that are gases at atmos-
pheric temperature aad pressure.
Non I—The procedure! described ia this
method may also fuid application ia sampling most
ooncorrosive liquid industrial chemical*, provided
that ail safety precautions specific to these chemicals
can be stnctly followed.
Non 2—The procedure for sampling liquefied
petroleum ga»es is described in ASTM Method
0 1263. Sampling Liquefied Petroleum (LP> Cases.'
the procedure for sampling electrical insulating oils
in ASTM Method O 923. Sampling Electrical Insu-
lating Otis.] and the procedure for sampling fluid
power hydraulic fluids is covered under ANSI/
B93 19 and ANS1/B93.44.
1.2 This procedure also coven sampling of
erode petroleum and aonumform petroleum
stocks and shipments. However, different de-
grees of uniformity or the presence of sediment
aad wtttr an shown to present manual sam-
ptindUBcolties that may affect the repnsent-
atMpHare of final samples.
II Sampling certain products requires a due
amount of caution for their handling. Refer to
Annex Al for precautionary sutcmenu regard-
ing thes* products.
3. Appekahte Documents
3.1 ASTM Standards:
D2I6 Method for Distillation of Natural
Gasoline*
D244 Methods of Testing Fmuiprjyf
Asphalts'
D268 Methods of Sampling and Testing Vol-
atile Solvents and Chemical Intermediates for
Use in Paint and Related Coatinp and Materials4
D323 Test Method for Vapor Pressure of Pe-
troleum Products (Reid Method)2
O 346 Methods for Collection and Preparation
of Coke Samples for Laboratory Analysis1
D525 Test Method for Oxidation Stability of
Gasoline (Induction Period Methodr1
D873 Tea Method for Oxidation Stability of
Aviation Fuels (Potential Residue MethodH
D977 Specification for Emulsified Asphalt1
01856 Test Method for Recovery of Asphalt
from Solution by Abson Method'
O2172 Test Method for Quantitative Extrac-
tion of Bitumen from Bituminous Paving
Mixtures'
4. StflMnary of Practice
4.1 A basic sampling method is available:
lank sampling, which is covered in this practice.
ts» juradicao*) of ASTM Coaautu*
'That
021
Cu
1911.
' /(wo* took of ASTM &«•*•*!. Vol 05.01.
1 Am* fa* of ASTM iMwtontt. Vol 04.03.
ItotttfASTMSie**!. Vol 06.01
IJbrtc tfASTtt Su^rn*. Vol 05.05.
-------
9951 .1
4 I.I [f the lank contents are not homoge-
neous from top to bottom of the tank or if the
conditions ui 4.1.2 are not met. automatic sam-
pling is recommended.
4.1.2 Tank samples will be representative if
the tank contents are homogeneous from top to
bottom. This is rarely the case to actual prac-
tice. However, tack samples are acceptable if
all of the following conditions prevail*
4.1.2.1 The tank contains a heavy compo-
nent (such as water) that clearly separates from
the mam component; and
4.1.2.2 The task i* equipped with either a
swing suction or a weir on the outlet that
prevents any shipment of the heavy compo-
nent: and
4.1.2.3 The tank samples are taken so that
none of the heavy component is included.
4.1.3 See Section 8 for additional precau-
tions and instructions.
5. SifaMcaaceaadUse
5.1 Samples of petroleum and petroleum
products are examined by various methods of
test for the determination of physical and
chemical characteristics. The test results are
often used for custody transfer and pricing
determinations. It is accordingly necessary that
the samples be representative of the petroleum
or petroleum products in question. The precau-
tions required to ensure the representative char-
acter of the samples are numerous and depend
upon the type of material being sampled, the
(jink, carrier, container or line from which the
sample is being obtained, the type and cleanli-
ness of the sample container, and the sampling
procedure that is to be used. A summary of the
sampling procedures and their application is
presented in Table I. Each procedure is suitable
for sampling a number of specific materials
under definite storage, transportation, or con-
tainer conditions. The basic principle of each
procedure is to obtain a sample or a composite
of several samples in such manner and from
such locations Jit the tank or other container
that the samplr or composite will be truly
repratautive of the petroleum or petroleum
product.
& Description ef Tern*
6.1 S0*pi*x
6.1.1 uniform pttnfaim product—one in
which spot samples from top. upper, middle,
lower, aad outlet agree wuhin^he precision of
04057
the laboratory tests. Similarly, in pipeline trans-
fers, spot samples taken at I. 20. 50. and 30 "-
of the total volume agree wuhin the precision
of the laboratory tests.
6.1.2 "official" sample—a sample taken it
the point of custody transfer and used for tne
custody transfer laboratory determination.
6.1.3 representative sample— a sample repre-
senting a small portion of its total volume of
material (for example, tanks, ships, compart-
ments, containers, and pipeline tenders* ob-
tained with a precision equal to or better thin
the precision of the laboratory method by
which this sample is to be analyzed.
6.1.4 all-levels sample—a sample obtained
by submerging a stoppered beaker or bottle to
a point as near as possible to the draw-off level
then opening the sampler and raising it at a
rate such that it is about three-fourths full
(maximum 85 %) as it emerges from the liquid.
An all-levels sample is not necessarily a repre-
sentative sample because the tank volume may
not be proportional to the depth and because
the operator may not be able to raise the sam-
pler at the variable rate required for propor-
tionate filling. The rate of filling is proportional
to the square root of the depth of immersion.
NOTI 3—The tubt sampling procedure. 953 may
be used to obtain an all-levels sample from a barrel
or drum.
6.1.5 running sample—a sample obtained by
lowering an unstoppered beaker or bottle from
the top of the oil to the level of the bottom of
the outlet connection or swing line, and return-
ing it to the top of the oil at a uniform rate of
speed such that the beaker or bottle is about
three-fourths full when withdrawn from the oil.
A running sample is not necessarily a repre-
sentative sample because the tank volume may
not be proportional to the depth and because
the operator may not be able to raise the sam-
pler at the variable rate required for propor-
tionate filling. The rate of Tilling is proportional
to the square root of the depth of immersion.
6.1.6 jpet sample— a sample taken at a spe-
cific location in tank or from a pipe at a specific
time during a pumping operation.
6.1.7 top sample—IL spot sample obtained 6
in. (152 nun) below the top surface of the liquid
(Fig. I).
6.1.3 upptrsampb—t spot sample taken at
the mid-point of the upper third of the tank
contents (Fig. I).
6.1.9 mtddle sample— a spot sample obtained
-------
from the middle of the tank contents (a point
halfway between the upper and lower sample
points) (Fig. 1). (See 9.3.2.)
6.1.10 lower sample—a spot sample obtained
at the mid-point of the lower third cf the tank
contents(Fig. I).
6.1.11 clearance sample—a spot sample
taken 4 in. (102 mm> below the level of the
tank outlet.
6.1.12 bottom sample—a sample obtained
from the material on the bottom surface of the
tank or container at its lowest point.
6.1.13 drain sample—a sample obtained
from the water draw-off valve. Occasionally, a
drain sample may be the same as a bottom
sample, as in the case of a tank car.
6.1.14 outlet tamplf—a spot sample taken at
the level of the bottom of the tank outlet (either
fixed or swing pipe) but not higher than one
meter above the bottom of the tank (see Fig.
1).
6.1.15 automatic sampler—a sampler used to
retrieve a representative sample from the liquid
flowing in a pipe. The automatic sampler gen-
erally consists of a probe, an extracting mech-
anism, an associated controller, and a sample
receiver.
6.1.16 single-tank composite sample—a
blend of the upper, middle, and lower samples.
For a tank of uniform cross section, such as an
upright cylindrical tank [he blend consists of
equal pans of the three samples. For a horizon-
tal cylindrical tank, the blend consists of the
three samples to (he proportions shown tn Ta-
ble 2.
6.1.1? multiple tank composite sample (ships,
barges, etc.)—a mixture of individual samples
from the several compartments each of which
contains the same grade of petroleum matenal.
The mixture is blended in proportion to the
volume of material in each compartment.
6.1.18 composite spot sample—a blend of
spot samples mixed volumetncally propor-
tional for testing. Some tests may also be made
oa the spot samples before blending and the
results avenged. Spot samples from crude oil
tanks an collected as follows:
6.1.18.1 Utnt-wav— On tanks larger than
1000-barrel capacity that contain in excess of
15 ft (4.6 m) of oiL equal-volume samples
should be taken at the upper, middle, and lower
or outlet connection of the merchantable oil in
the order named. On tanks of 1000-barrel ca-
04057
pacuy and less, this method may also be used.
6.1.18.2 two-way— On tanks larger than
1000-barrel capacity that contain in excess of
10 ft (3.0 m) and up to 15 ft ,46 m) of oil
equal-volume samples should be taken at the
upper and lower, or outlet, connection of (he
merchantable oil. in the order named. On tanks
of 1000-barrel capacity and under, this method
may also be used.
6.1.19 middle spot sample—On tanks larger
than 1000-barrel capacity containing 10 ft [30
m> or less of crude oil. one spot sample should
be taken as near the center of the vertical
column of oil as possible and outlet connection.
6.1.20 dipper sample—a sample obtained by
placing a dipper or other collecting vessel into
the path of a free-flowing stream so as to collect
a definite volume from the full cross section of
the stream at regular tune intervals for a con-
stant rate of flow, or at time intervals vaned in
proportion to the rate of flow
6.1.21. tube or thief sample—a sample ob-
tained with a sampling tube or special thief.
either as a core sample or spot sample from a
specified point in the tank or container
6.1.22 tank-side sample—a spot sample
taken from a sample connection in the side of
a tank.
6.1.23 surface sample—a spot sample
skimmed from the surface of a liquid in a tank.
6.1.24/701* proportional sample—a sample
taken from a pipe during the entire transfer.
The rate of sampling is proportional to the flow
of the liquid in the pipe at any instant.
. 6.1.23 entrained water—water suspended in
the oil, Entrained water includes emulsions but
does not include dissolved water.
6.1.26 free water—water that exists as a sep-
arate phase and typically lies beneath the oil.
6.1.27 emulsion—an oil/water mixture that
does not readily separate.
6.1.28 sample receiver /receptacle>—i con-
tainer in which all sample bites are collected
during sampler operation. A receiver may be
fixed or portable.
6.1.29 bonnes sample—a sample obtained
by collecting the chips made by boring holes
with a ship auger from top to bottom of the
material contained in a barrel, case. bag. or
cake.
6.1.30 grab sample—* sample obtained by
collecting loose solids in equal quantities from
each pan or package of a shipment and in
-------
sufficient amount to be characteristic of all sizes
and components.
6. 1.3 1 grease sample — a sample obtained by
scoopuig or dipping a quantity of soft or sem-
iliquid material, such u grease, from a package
in such a manner that the material on the scoop
or dipper is representative of the material in
the package.
7. Apparatus
7.1 Sample Containers may be clear or
brown glass bottles, or cans. The clear bottle is
advantageous because it may be examined vis-
ually for cleanliness, and also allows visual
inspection of the sample for free water or solid
impurities. The brown glass bottle affords some
protection from light. The only cans permissi-
ble are those with the seams soldered on the
exterior surfaces with a flux of rosin in a suit-
able solvent. Such a flux is easily removed with
gasoline, whereas many others are very difficult
to remove. Minute traces of flux may contam-
inate the sample so that results obtained on
tests for dielectric strength, resistance to oxi-
dation. and sludge formation may be erro-
neous.
7. 1 . 1 Plastic Bottles made of suitable unpig-
mented linear polyethylene may be used for
the handling and storage of gas oil diesel oil.
fuel oil. and lubricating oil. They should not be
used for gasoline, aviation jet fuel kerosine.
crude oil. white spirit, medicinal white oil. and
special boiling point products unless testing
indicates there is no problem with solubility.
contamination, or loss of light ends.
NOTE 4— In no circumstances shall nonlinear
(conventional) polyethylene containers be used to
store samples of liquid hydrocarbons. Ton u to avoid
sample contamination of sample bottle failure. Used
engine-toil samples thai may have been subjected to
fuel diluiioa should not be stored in plastic con-
tainers.
Non 5— Plastic bottles bave an advantage. They
will not shatter lite glass or corrode like metal con-
tainers. They are generally used only once and then
discarded so that radcaaatg and recovery procedures
an not required.
7.2 Container C/oJurr— Cork or glass stop-
pen, or screw caps of plastic or metal, may be
used for glass bottles: screw caps only shall be
used for cans to provide a vaponight closure
seal Corks must be of good quality, clean, and
AM of holts and. loose bits of cork. Never use
rubber stoppers. Contact of the sample with the
cork may be prevented by wrapping tin or
aluminum foil around the cork before forcinj
it into the bottle. Glasi stoppers must be j
perfect fit. Screw caps must be protected by j
disk faced with tin or aluminum foil, or other
material that will not affect petroleum or petro-
leum products.
7.3 Cleaning Procedure—All sample con-
tainers must be absolutely clean and free of
water, din. lint, washing compounds, naphtha.
or other solvents, soldering fluxes or acids,
corrosion, rust, or oil. Before using a container.
rinse it with Stoddard solvent or other naphtha
of similar volatility. (It may be necessary'to use
sludge solvents to remove all traces of sediment
and sludge from containers previously used.)
Then wash the container with strong soap so-
lution, rinse it thoroughly with tap water, ud
finally wuh distilled water. Dry either by past-
ing a current of clean, warm air through toe
container or by placing it in a hot dust-free
cabinet at 40°C (104°F) or higher. When dry,
stopper or cap the container immediately. In
the ordinary field sampling of crude petroleum.
washing with soap and rinsing with water may
be eliminated.
7.4 Sampling Ca$e—This shall be a metal or
plastic holder or cage, suitably constructed to
hold the appropriate container. The combined
apparatus shall be of such a weight as to sink
readily in the material to be sampled, ud
provision shall be made to fill the container at
any desired level (see Fig. 2a). Bottles of special
dimensions are required to fit a sampling cage.
The use of a sampling cage is generally pre-
ferred to that of a weighted sampling beaker
for volatile products since loss of light ends is
likely to occur when transferring the sample
from a weighted sampling beaker to another
container.
7.5 Sampling Apparatus is described in detail
under each of the specific sampling procedures.
Sampling apparatus shall be clean, dry. ud
free of all substances that might contaminate
the material.
8. PrccMdoos and Instructions
8.1 Crude Petroleum and Heavy Fuel Oil:
usually are nonhomogeneous. Automatic sam-
plers are recommended for sediment and water
(SAW) and density measurement.
8.1.1 Tank samples may not be representa-
tive because:
-------
8.1.1.1 The concentration of entrained water
is higher near the bottom. The running sample
or the composite of the upper, middle and
lover sample may not represent the concentra-
tion of entrained water.
3.1.1.2 The interface between oil and free
water is difficult to measure, especially in the
presence of emulsion. layers, or sludge.
8.1.1.3 Determining the vol ume of free water
is difficult because the free water level varies
across the tank bottom surface. The bottom is
often covered by pools of free water or water
emulsion impounded by layers of sludge or
wax.
8.2 Gasoline and Distillate Products usually
are homogeneous but they are often shipped
from tanks that have clearly separated water
on the bottom. Tank sampling is acceptable
under the conditions covered in 4.1.2.
8.3 When using tank samples, the SAW de-
duction is usually the sum of the free water
volume (usually determined from a paste cut)
and the entrained water volume determined
from the SAW analysis of the tank sample. The
difficulty of determining the free water volume
limits the accuracy of the S&W deduction.
8.3.1 Automatic samplers are recommended.
However, by mutual agreement, shore tanks.
ship's compartment or manual line samples
may be used.
8.4 Sample Handling and Dividing of Crude
Petroleum and Sonuinform Products:
8.4.1 The transfer of crude oil samples from
the sample receiver to the laboratory glassware
in which they will be analyzed requires special
care to maintain their representative nature.
The number of transfers should be minimized.
Mechanical means of mixing and transferring
the samples an recommended. An external
circulating system provided with pump and in-
line mixing element that couples directly to the
sample container is one method. Mixing time
and flow rates an critical in such systems. A
•tor that is inserted in the sampler container
it another method. Whatever handling, divid-
aad mixing system is chosen, however, its
pvfonaanc* should be verified by introducing
•ad mastering samples of known water con-
centration.
8.4.2 In mixing and transferring representa-
tive samples. th* variation from known water
concentration should not exceed x 0.05 % when
the known water concentration is I % or less
04057
and * 5 "e of the known water concentration
when a is over I et.
8.5 Marine Custody Transfer—By mutual
agreement, samples can be taken from shore
tanks, from ship's tanks, or from pipelines.
Pipeline samples may be taken automatically
or manually. Properly taken automatic pipeline
samples are the most representative. Manual
pipeline samples are less representative than
automatic pipeline samples. Manual pipeline
sampling is described in 94. Tank samples will-
usually not be representative unless (he tank is
completely homogeneous and contains no free'
water.
8.5.1 Stationary or Shore Tanks:
8.5.1.1 Crude petroleum tanks may be sam-
pled in the following ways by mutual agree-
ment: composite spot, middle spot, all-levels.
running samples or by sample cocks. Addi-
tional samples may be taken as necessary.
Norc 6—Where emulsions ire in relatively higher
concentration in the bottom portions of the link, ibe
lower simple would not be considered representative
of this lower third. Automatic line sampling u rec-
ommended in such cases, (f this is not possible an
outlet sample or bottom sample should be required
instead of the lower sampled In addition, a bottom
thieving should be made for both opening and closing
gauges so that any change in the SAW level at :be
bottom of the tank may be observed and noted.
8.5.1.2 Where tank samples must be used for
crude oil fucalization and the tanks do not
have swing suction lines or weirs, it ts recom-
mended that upper, middle, and outlet samoies
be taken. These samples should be tested and
reported separately. The S&W deduction
should be the average of the three values. Other
analyses should also be averaged.
8.5.2 Ship or Barge Transfers— Samples of
ship cargoes of crude petroleum may be taken
by the following methods by mutual agreement:
8.5.2.1 From the shore tanks before loading
and both before and after discharging as pre-
viously described,
8.5.2.2 From the pipeline during discharging
or loading. Pipeline samples may be taken
either manually or with an automatic sampler
If the pipeline requires displacement or flush-
ing, care must be taken that the pipeline sample
includes the enure cargo and none of the dis-
placement Separate samples may be required
to cover the effect of the line displacement on
the prior or following transfer.
8.5.2.3 From the ship's tanks after loading
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04057
or before discharging. An all-levxis sample or
a running sample shall be obtained from each
compartment of the ship's cargo tanks.
8.5.2.3 (/) Except where specifically ex-
empted, when loading a ship, the shore tank
sample or the pipeline sample taken from the
loading line shall be official. However, ship's
tank samples may also be tested for sediment
and water, and for other quality aspects when
required. The results of these ship's tank sample
tests, together with the shore tank sample tests.
may be shown on the cargo certificate.
8.5.13 (7) When discharging a ship, the
pipeline sample taken from a properly designed
and operated automatic line sampler in the
discharge line shall be official. Where no
proper line sample is available, the ship's tank
sample will be official except where specifically
exempted.
8.6 Finished Proaucts—When loading or dis-
charging finished products, take samples from
both shipping and receiving tanks, and from
the pipeline if required.
8.6.1 Ship or Barge Tanks—Simple each
product after the vessel is loaded or just before
unloading.
8.6.2 Tank Car*—Sample the product after
the car is loaded or just before unloading.
8.6.3 Package Lots (Cans. Drums. Barrels, or
Boxesi—Take samples from a sufficient num-
ber of the individual packages to prepare a
composite sample that will be representative of
the enure lot or shipment. Select at random the
individual packages to be sampled. The num-
ber of such random packages will depend upon
several practical considerations, such as:
8.6.3.1 The tightness of the product specifi-
cations;
8.6.3.2 The source and type of the material
and whether or not more than one production
batch nay be represented in the lot: and
8.6.3.3 Previous experience with similar
shipments, particularly with respect to the uni-
formity of quality from package to package.
8.6.4 la most cases, the number specified in
Table 3 will be satisfactory.
8.7 Obtaining Samples:
8.7.1 Extreme care and good judgment are
necessary to ensure samples are obtained that
represent the general character and average
condition of the maimal Clean hand* are
important. Clean gloves may be worn but only
when absolutely necessary, such as in cold
weather, or when handling matenals ai a huh
temperature, or for reasons of safety Select
wiping cloths so that lint is not introduced.
which would contaminate samples. ,
8.7.2 As many petroleum vapors are toxic
and flammable, avoid breathing them or ignit-
ing them from an open flame or a spark pro-
duced by static. Follow all safety precautions
specific to the material being sampled.
8.7.3 When sampling relatively volatile
products (more than 2 psi 1133 kPai Rvpi. Fdl
and allow the sampling apparatus to drain
before drawing the sample. If the sample is to
be transferred to another container, also nnse
this container with some of the volatile product
and then drain. When the actual sample is
emptied into this container, upend the sam-
pling apparatus into the opening of the sample
container and allow to remain in this position
until the contents have been transferred so thar
no unsaturated air will be entrained in the
transfer of the sample.
8.7.4 When sampling nonvolatile liquid
products (2 psi (13.8 kPa) Rvp or less), the
sampling apparatus shall be filled and allowed
to drain before drawing the actual sample. If
the actual sample is to be transferred to another
container, rinse the sample container with some
of the product to be sampled and drain before
it is filled with the actual sample.
NOT* 7—When taking samples from tanks sus-
pected of containing flammable atmospheres, precau-
tions should be taken to guard against ignitions due
to static electricity Metal or conductive ootec-.s such
u gage tapes, sample containers, and thermometers.
should not be lowered into or suspended m. i com-
panmtat or taak which is being filled or immediately
after ctuauon of pumping. A waning period will
generally permit a substantial relaxation ot ihe eiec-
irtnuuc charge.
8.8 Handling Samples:
8.8.1 Volatile Samples—h is necessary to
protect all volatile samples of petroleum and
petroleum products from evaporation. Transfer
the product from the sampling apparatus to -.he
sample container immediately. Keep the con-
tainer closed except when the matenal is being
transferred. When samples of more than 16 psi
(110 kPa) Rvp are being obtained, be sure to
use containers strong enough to meet local
safety regulations. After delivery to the labo-
ratory, volatile samples should be cooled beiore
the container is opened.
8.8.2 Light-Sensune Samples— It is impor-
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04057
tarn thai samples sensitive to light, such as
gasoline containing tetraethyllead. be kept in
the dark, if the testing is to include the deter-
mination, of such properties as color, tetra-
ethyJIead and inhibitor contents, sludge-form-
ing characteristics, stability tests, or neutrali-
zation value. Brown glass bottles may be used.
Wrap or cover clear glass bottles immediately.
It is a definite advantage to use covered card-
board canons into which the sample bottles
may be placed immediately after collection.
8.8.3 Refined Materials—Protect highly re-
fined products from moisture and dust by plac-
ing paper, plastic or metal foil over the stopper
and the top of the container.
8.8.4 Container Outage—Never completely
fill a sample container, but allow adequate
room for expansion, taking into consideration
the temperature of the liquid at the time of
filling and the probable maximum temperature
to which the filled container may be subjected.
8.9 Shipping Samples—To prevent loss of
liquid and vapors during shipment, and to pro-
tect against moisture and dust, cover the stop-
pers of glass bottles with plastic caps that have
been swelled in water, wipe dry. place over the
tops of the stoppered bottles, and allow to
shrink tightly in place. Screw the caps of metal
containers down tightly and check for leakage.
Appropriate regulations applying to the ship-
ment of flammable liquids must be observed.
8.10 Labeling Sample Containers:
8.10.1 Label the container immediately after
a sample is obtained. Use waterproof and oil-
proof ink or a pencil hard enough to dent the
tag. since soft pencil and ordinary ink markings
are subject to obliteration from moisture, oil
smearing, aad handling. Include the following
information:
8.10.1.1 Date aad time (the penod elapsed
during continuous *^" Rvp or less in tank
cars, tank trucks, shore tanks, ship tanks, and
barge tanks. Solids or semiliquids that can be
liquefied by heat may be sampled by this pro-
cedure, provided they are true liquids at tune
of sampling.
9.2.2 Apparatus—A suitable sampling bottle
or beaker, as shown in Fig. 1 is required.
Recommended uses and diameter of openings
in the bottle or beaker are given in Table 4.
9.2.3 Procedure:
9.2.3.1 All-Levels Sample (One-Way)—
Lower the weighted, stoppered bottle, or beaker
as near as possible to the draw-off level pull
out the stopper with a sharp jerk of the line and
raise the bottle at a uniform rate so thai it is
about three-fourths full as it emerges from the
liquid. For light products or deep tanks, a
restricted opening may be needed to avoid
filling the bottle.
9.2.3.2 Running Sample (Two-Wjy)—
Lower the unstoppered bottle or beaker as near
as possible to the level of the bottom of the
outlet connection or swing line and then raise
the bottle or beaker to the top of the oil at a
uniform rate of speed such that it is about
three-fourths full when withdrawn from the oil.
For light products or deep tanks, a notched
cork or other restncted opening may be needed
to avoid filling the bottle.
9.2.3.3 Top, Upper. Middle. Lower and Outlet
Samples—Lower the weighted, stoppered bot-
tle to the proper top. upper, middle, lower, and
outlet depths.(see Fig. I).
NOTI 8—Where emulsions are in relatively higher
concentration in the bottom portions of the tank. :ne
lower sample would not be considered representative
of this lower third. Automatic line sampling is rec-
ommended in such ca*es. If ibis is not possible in
outlet sample or bottom sample should be requircc
instead of the lower sample. In addition, mate t
bottom thieving for both opening aad closing gage*
so thai any change in the S«W level at the bottom ot
the tank may be observed aad noted.
9.2.3.3(1) At the selected level pull out :ne
stopper wuh a sharp jerk of the line and allow
the bottle or beaker to fill completely When
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3SVER 9931.1
judged full, raise ihe bottle or beaker, pour off
a small amount, and stopper immediately.
9 2.3 3(2) Where tank samples must be used
for crude oil fiscalization and the tanks do not
have swing suction lines or weirs, it is recom-
mended that upper, middle, and outlet samples
be taken. Test these samples and report sepa-
rately. The SAW deduction should be the av-
erage of the three values. Also average other
analyses.
9.2.3.4 Multiple Tank Composite Sample—
Prepare a composite sample in the laboratory
(not in the field) by mixing portions of the all-
levels samples as specified in 6.1.16.
9.2.3.5 Composite Spot Sample—Prepare a
composite spot sample by mixing spot samples
in equal proportions as specified in 4.1.18. using
either the three-way or the two-way procedure.
whichever applies.
9 2.3.6 Middle Spot Sample— Obtain this
sample in the manner specified in 6.1.19.
9 2.3.7 Handling—Stopper and label bottle
samples immediately after taking them, and
deliver to the laboratory in the original sam-
pling bottles. There is an advantage to using a
bottle and a sampling cage instead of a
weighted beaker for volatile products. The loss
of light ends is likely to occur when transferring
the sample from a weighted beaker to another
container.
9.3 Tap Sampling:
9.3.1 Application—The tap sampling proce-
dure is applicable for sampling liquids of 26 psi
11 ?9 kPa> Rvp or less in tanks that are equipped
wuh suitable sampling taps or lines. This pro-
cedure is recommended for volatile stocks in
tanks of the breather and balloon-roof type.
spheroids, etc. (Simples may be taken from the
draw cocks of gage glasses, if the tank is not
equipped with sampling taps.) The assembly
for tap sampling is shown in Fig. 3.
lOkPaibui
bath u
, fton *— If Rvp is morethan I6psi(ll0l
JMrfcore than 26 p*i (ImkPai. a cooling
M IB Fig. 10 shall be used between the tank tap
fllM sample container to cool the sample and
' and prevent volatilization of low-boiling
9.3.2 Apparatus:
9.3.11 Tank Taps—The tank should be
equipped with at least three sampling taps
placed equidistant throughout the tank height
and extending at least 3 ft (0.9 mi inside the
tank shell. A standard H in. pipe wuh suitable
04057
valve is satisfactory.
9.3.2.2 Sample Cocks— Samples of crude pe-
troleum may be taken through sample cocks
properly placed in the shell of the tank. The
upper sample cock shall be located 18 in. (457
mm) below the top of the tank shell: the lower
sample cock shall be located level wuh the
bottom of the outlet elbow or other similar
fitting if installed on the outlet connection: and
the middle sample cock shall be located half-
way between the upper and lower sample cocks.
An additional cock for the clearance sample
should be located 4 in. (102 mm) below the
bottom of the outlet connection to determine
whether the level of merchantable oil is at least
below this point. The sample cocks should be
located a minimum of 6 ft (1.3 m) distant
circumferenually from the pipeline outlet and
drain connection or at the top of upturned
connections, and 8 ft (2.4 m) from the Tilling
line connection. The sample cocks should be of
V4 in. size, and the lines should be of *« in.
nominal diameter for crude oil of 18° API
gravity or less. For lighter oiL -7-in. size cocks.
with W-in. nominal diameter lines, should be
used. The lines should extend a minimum of 4
in. (102 mm) inside the tank shell, except on
floating-roof tanks, where flush installations
are necessary. All sample cocks should be
equipped with scalable valves and plugged in-
spection tees.
9.3.2.211) On tanks of more than 10 000-
barrel capacity, at least two sets of sample cocks
shall be installed, located equidistant around
the circumference of the tank. Five or more
sample cocks should be installed per set. even!)
spaced between lower and upper sample levels
9.3.2.3 Tube— A delivery tube that will not
contaminate the product being sampled and
long enough to reach to the bottom of ;he
sample container is required to allow sub-
merged filling. When a cooling bath is used
while tap sampling, a similar suitable tube
should be used between the tank tap and the
cooler inlet
9 3.2.4 Sample Containers— Use clean, dr-
glass bottles of convenient size, and strength :o
receive the samples. If the vapor pressure of the
product to be sampled is between 16 and 26 pi
(110 and 179 kPa> Rvp. protect the bottle <*nn
a metal cover until the sample is discarded I n
some cases, such as the sampling of cruce
petroleum, metal containers may be used •_-.
-------
04057
stead of glass bottles.
9 3.3 Procedure:
9.3.3.1 Before a sample is drawn, flush the
tap tor gage glass drain cock) and line until
they are purged completely Connect the clean
delivery tube to the tap. Draw upper, middle.
or lower samples directly from the respective
taps after the flushing operation. Stopper and
label the sample container immediately after
filling, and deliver u to the Laboratory.
9.3.3.2 When a sample cooler is used during
the tap sampling operation, flush the tap (or
gage glass drain cock). Then, using a section of
clean tubing, connect the tap to the cooler inlet.
Flush the cooler thoroughly, after which con-
nect the clean delivery tube to the cooler outlet
and proceed with the sampling operation.
9.3.3.3 In the sampling of crude petroleum.
check for merchantable oil at the clearance
sample cock. Flush each sample connection
until all oil from the previous run has been
removed and the sample lines are filled with
fresh oil from the tank.
9 3.3.3(7) On tanks of 10 000-barrel capac-
ity or smaller, take samples of equal amounts
from the lower, middle, and upper sample con-
nections. A measuring cup of proper size may
be used to assure the drawing of the proper
quantity from each sample cock.
9.3.3.3(2) On tanks of more than 10 000-
barrel capacity, take samples of equal amounts
from each of the sample connections at each set
of sample connections.
9 3.3.3(J) Mix all samples in equal propor-
tions for a composite sample, or test the samples
separately and average the results.
9.3.3.3(4) When crude oil in a tank fails to
reach the upper ox middle sample cocks on a
tank equipped with three sample cocks, it is
suggested that the sample for the run be ob-
tained at follows: if the level of the oil is nearer
law upper sample cock than the middle, take
two thirds of the sample from the middle sam-
cock aad oac third from the lower. If the
of oiJ is nearer the middle sample cock
the upper, uiur one half of the sample
from the middle and one half from the lower.
if the level of the oil is below the middle sample
cock, take alt of the sample from the lower
cock.
9.4 Manual Sampling of Pipeline Streams:
9.4.1 Application—This manual Kne sam-
pling procedure is applicable for sampling liq-
uids of 16 psi 1110 kPai Rvp or less and semi-
liquids in pipelines, filling lines, and transfer
lines. Where custody transfer is involved, con-
tinual automatic sampling is the preferred
method. In the event of automatic sampler
failure, manual samples may be needed. Take
such manual samples as representatively as pos-
sible.
9.4.2 Apparatus:
9 4.2.1 Sampling Probe—The function of :he
sampling probe is to withdraw from the (lowing
stream a portion that will be representative of
the entire stream. Probe designs that are com-
monly used are shown in Fig. 4. These are:
94.2.1(7) A tube extending to the center of
the line and beveled at a 45" angle facing
upstream i Fig. 4
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>. -..-.-.
' - A ~. A
3 C "
1 . 1
ceptable level. If flow has been vertical for a
sufficient distance as in a platform nser. such
a device may not be necessarv even at low-flow
rates. Some effective deuces for obtaining ad-
equate mixing are: a reduction in pipe size: a
senes of baffles: an orifice or perforated plate:
or a combination of any of these methods. The
design or sizing of the device is optional with
the user, as long u the flowing stream is suffi-
ciently well mued to provide a representative
sample from the probe.
9 4 3(.<) The sampling point should be as
near as practicable to the pouit where the oil
passes to the sample receiver.
9 4.3
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9951.1
psi (13.8 kPa) Rvp or less and semiliquids in
drums, barrels, and cans.
9 6.2 Apparaiur.
96.2.1 Tubt—Enher a glass or metal tube
may be used, designed so (hat it will reach to
within about •» in. (3.2 mmi of the bottom and
have a capacity of approximately I pt (0.5 L)
or I qt (0.9 L). A metal tube suitable for
sampling 50 gal (190 L) drums is shown in Fig.
5. Two rings soldered to opposite sides of the
tube at the upper end are convenient for hold-
ing it by slipping two fingers through the rings.
thus leaving the thumb free to close the open-
ing.
96.2.2 Sample Containers—Use clean, dry
cans or glass bottles.
96.3 Procedurr.
9.6.3.1 Drum* and Barrels—Place the drum
or barrel on its side with the bung up. If the
drum does not have a side bung, stand it up-
right and sample from the top. If detection of
water, nut. or other insoluble contaminants is
desired, let the barrel or drum remain in this
position long enough to permit the contami-
nants to settle. Remove the bung and place it
beside the bung hole with the oily side up.
Close the upper end of the clean, dry sampling
tube with the thumb, and lower the tube into
the oil for a depth of about 1 ft (0.3m). Remove
the thumb, allowing oil to flow into the tube.
Again close the upper end with the thumb and
withdraw the tube. Rinse the tube with the oil
by holding it nearly horizontal and turning it
so that the oil comes in contact with that pan
of the inside surface that will be immersed
when the sample is taken. Avoid handling any
pan of the tube that will be immersed in the oil
during the sampling operation. Discard the
rinse oil and allow the tube to drain. Insert the
tube into the od again, holding the thumb
against the upper end. (If an all-levels sample
is desired, insert the tube with the upper end
open.) When the tube reaches the bottom, re-
move the thumb and allow the tube to fill.
Replace toe thumb, withdraw the tube quickly.
aad transfer the contents to the sample con-
tainer. Do not allow the hands to come in
contact with any pan of the sample. Close the
sample container replace and tighten the bung
in the drum or barrel Label the sample con-
tainer and deliver it to the laboratory.
9.6.3.2 Cow—Obtain samples from cans of
04O57
5-gal (19-L) capacity or larger in the same
manner as from drums and barrels (96.3.it.
using a tube of proportionately smaller dimen-
sions. For cans of less than 5-gal (19-L) capac-
ity, use the entire contents as the sample, se-
lecting cans at random as indicated in Table 3
or in accordance with agreement between the
purchaser and the seUer.
9.7 Thief Sampling.
9.7.1 Application: The thief sampling proce-
dure is applicable for obtaining boiiora samples
(Fig. I), or of semiliquids in tank cars and
storage tanks.
9.7.1.1 The thief is also widely used in sam-
pling crude petroleum in storage tanks. In this
application it may be used for taking samples
at different levels as well as for bottom samples
of nonmerchantableotl and water at the bottom
of the tank.
9.7.3 Apparatus:
9.7.3.1 Thitf— The thief shall be designed so.
that a sample can be obtained within 4 in. (13
mm) of the bottom of the car or tank. Two
types of thiefs are illustrated in Fig. 6. One type
is lowered into the tank with valves open to
permit the oil to flush through the container
When the thief stakes the bottom of the tank.
the valves shut automatically to trap a bottom
sample. The other type has a projecting stem
on the valve rod which opens the valves auto-
matically as the stem strikes the bottom of the
tank. The sample enters the container through
the bottom valve and air is released simulta-
neously through the top. The valves snap shut
when the thief is withdrawn. A core-type thief
similar to that shown in Fig. 6<&). with a uni-
form cross section and bottom closure and with
a capacity depending upon the size of the sam-
ple required, may be used for sampling crude
petroleum. The thief should be capable of pen-
etrating the oil in the tank to the required level.
mechanically equipped to permit filling at any
desired level, aad capable of being withdrawn
without undue contamination of the contents
The thief may be equipped with the following.
9.7.3.1 (/) Sample cocks for obtaining sam-
ples for the determination of water and sedi-
ment;
9.7.3.1 (2) Extension rods for use in obtain-
ing samples at levels corresponding with re-
quirements for high connections or for samples
II
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040S7
to determine high settled water and sediment
levels:
9 7.3. | f J) Water and sediment gage for de-
termining the height of water and sediment in
the thief:
9.7 3.1 (4) Windshield to be used when tak-
ing the gravity and temperature of the oil:
9.7 3.1 (J) Opener to break the tension on
the valve or slide at any desired level:
9.7.3.1 (6) A thief cord marked so thai sam-
ple can be taken at any depth in the vertical
cross section of the tank: and
9.7.3.1 (7) Hook to hang the thief in the
hatch vertically.
9.73.2 Samplt Containers— Use clean, dry
cans or glass bottles.
9.7.4 Procedure
9 7.4.1 Lower the clean, dry thief through
the dome of the tank car or tank hatch until it
stnkes the bottom. When full, remove the thief
and transfer the contents to the sample con-
tainer. Close and label the container immedi-
ately, and deliver it to the laboratory.
9.7.4.2 In the sampling of crude petroleum
lower the clean, dry thief slowly into the oil to
the desired depth, trip the thief to secure the
sample and raise slowly to avoid agitation. The
proper depths for sampling are described in
4.1.
9.8 Boring Sampling:
9.8.1 Application—The boring sampling pro-
cedure is applicable for sampling waxes and
soft solids in barrels, cases, bags, and cakes
when they cannot be melted and sampled as
liquids.
9.8.2 Apparatus:
9.8.2.1 Ship Auger—Use a ship auger *i in.
(19 mm) in diameter, similar to that shown in
Fig. 7. and of sufficient length to pass through
the material to be sampled.
9.8.12 S'omplt Containers—Uxclean, wide*
mouth, metal containers or glass jars with cov-
en.
9.8.3 Procedure— Remove the heads or cov-
en of barrels and cases. Open bags and wrap-
pings of cakes. Remove any din. sticks, string.
or other foreign substances from the surface of
(he material. Bore three test holes through the
body of the material, one at the center, the
other two halfway between the center and the
edge of (he package on the right and left sides.
respectively. If any foreign matter is removed
from the interior of the material during the
bonng operation, include it as pan of ihe bor-
ings. Put the three sets of bonngs in individual
sample containers, label and d'ehver them to
the laboratory.
9.8.4 Laboratory Inspection—If there are
any visible differences in the samples, examine
and test each set of bonngs at the laboratory
Otherwise, combine the three sets of bonngs
into one sample. If subdivision of the bonngs
is desired, chili pulverize (if necessary), mix.
and quaner the bonngs until reduced :o the
desired amount.
9.9 Grab Sampling:
9.9.1 Application:
9.9.1.1 The grab sampling procedure is ap-
plicable for sampling all lumpy solids in bins.
bunkers, freight cars, barrels, bags, boxes, and
converyors. It is particularly applicable for the
collection of green petroleum coke samples
from railroad cars and for the preparation of
such samples for laboratory analysis. Refer to
Method O 346 when other methods of shipping
or handling are used.
9.9.1.2 Place of Sampling—Petroleum coke
may be sampled while being loaded into rail-
road can from piles or after being loaded into
railroad can from coking drums.
9.9.2 Apparatus:
9.9.2.1 Samplt Container—A polvethtlene
pail of approximately 10-qt (9.5-L) capacity
9.9.2.2 Scoop, stainless s:eel or aluminum.
No. 2 size.
9.9.3 Procedure.
9.9.3.1 Sampling— Lumpy solids are usuaJly
heterogeneous and therefore arc difficult to
sample accurately It is preferable to take sam-
ples during the unloading of cars, or during
transit of the matenal by conveyors. From ma-
terial in transit obtain a number of portions at
frequent and regular intervals and combine
t ft fin
9.9.3.2 Whea sampling from railroad cars.
use one of the following procedures.
9.9.3.2 (/) Being Loaded from a Pile—Tike
a full scoop of sample at each of the five
sampling points shown in Fig. 8 and deposit in
(he polyethylene pad. Cover the sample and
deliver to the laboratory. Each sampling point
shall be located equidistant from the sides of
(he railroad car.
9.9.3.2 (2) Railroad Can After Direct Load-
ing/mm Caking Drumt—At any five of the
sampling points shown in Fig. 9. take a full
12
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OSWER 9951.1
scoop of coke from about I ft (0.3 m) below
the surface and deposit a ui the polyethylene
pail. Cover the sample and deliver to the lab-
oratory
9.9.3.3 When sampling from conveyors, take
one scoop for each 8 to 10 tons (7 9 to 9 Mg) of
coke transported. These samples may be han-
dled separately, or composited after ail samples
representing the lot have been taken.
9.9.3.4 When sampling from bags, barrels.
or boxes, obtain pontons from a number of
packages selected at random as shown in Table
3. or in accordance with the agreement between
the purchaser and the seller
9.9.3.5 Quartering—Carefully mix the sam-
ple, and reduce it in size to a convenient labo-
ratory sample by the quartering procedure de-
scribed in Method D 346. Perform the quarter-
ing operation on a hard, clean surface, free
from cracks, and protected from rain. snow.
wind, and sun. Avoid contamination with cin-
ders, sand, chips from the floor, or any other
material. Protect the sample from loss or gain
of moisture or dust. Mix and spread the sample
in a circular layer, and divide it into quadrants.
Combine two opposite quadrants to form a
representative reduced sample. If this sample is
still too large for laboratory purposes, repeat
the quanenng operation. In this manner, the
sample will finally be reduced to a representa-
tive, suitable size for laboratory purposes. Label
and deliver the sample to the laboratory in a
suitable container. Subdivision may be made
in the laboratory by using a riffle sampler as
Method D 346. '
9.10 Great Sampling
9.1 O.I Application—This method coven
practices for obtaining samples representative
of production lots or shipments of lubricating
greases, or of soft waxes or soft bitumens similar
to grease in consistency. The procedure is nec-
essarily quite general to cover the wide variety
of conditions encountered, and may require
modification to meet individual specifications.
Proceed in accordance with 6.1 to 8.7. particu-
larly those pertaining to precautions, care, and
ckulineu. except where they conflict with
9.10.2 to 9.10.4.
9.10.2 Inspection:
9.10.Z1 If the material is a lubricating grease
and inspection is made at the manufacturing
plant, take samples from the finished shipping
containers of each production batch or lot
D4O57
Never take grease samples directly from grease
kettles, cooling pans, tanks, or processing
equipment. Do not sample the grease until it
has cooled to a temperature not more than
I5°F (8 39C) above that of the air surrounding
the containers and until it has been m tbe
finished containers for at least 12 h. When the
containers for a production batch of grease are
of different sizes, treat the grease in each tax
of container as a separate lot. When inspection
is made at the place of delivery, obtain a sample
from each shipment. If a shipment consists of
containers from more than one production
batch (lot numbers), sample each such batch
separately.
9.10.2.2 If the material being inspected is of
grease-like consistency, but is not actually a
lubricating grease, but some mixture of heavy
hydrocarbons such as microcrystailine waxes
or soft bitumens, it will be permissible to take
samples from pans, tanks, or other processing
equipment, as well as from containers of the
finished product. The grease sampling method
shall be applicable to such stocks only if for
some reason it is not possible to apply heat and
conven the material into a true liquid.
9.10.3 Sample Size—Select containers at
random from each lot or shipment to give the
desired quantity specified in Table 5
9.10.4 Procedure.
9.10.4.1 Inspection—Examine the opened
containers to determine whether the grease ts
homogeneous, comparing the grease nearest
the outer surfaces of the container with thai ui
the center, at least 6 in. (152 mm) below the
top surface, for texture and consistency When
more than one container of a lot or shipment
is opened, also compare the grease in the re-
spective containers.
9.10.4.2 Sampling—If no marked difference
in the grease is found, take one portion from
the approximate center and at least 3 in. (76
mm) below the surface of each opened con-
tainer, in sufficient quantity to provide a com-
posite sample of the desired quantity i Table 51.
Withdraw portions with a clean scoop. large
spoon, or spatula and place them in a clean
container. Very soft semifluid greases may be
sampled by dipping with a l-lb (045-kg) can
or suitable dipper. If aay marked difference u»
th* grease from the various locations of an
opened container is found, take two separate
samples of about I Ib (0.45 kg) each, one from
13
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OSWER 9951 .1
the top surface adjacent to the wall, and the
other from the center of the container, at least
6 in. (152 mm) below the top surface. If any
marked variations are noted between different
containers of a lot or shipment, take separate
samples of about 1 Ib (0.45 kg) from each
container. When more than one sample of a
batch or shipment is taken because of lack of
uniformity, send them to the laboratory as
separate samples.
9.10.4.3 Handling Samples—If more than
one portion is required to represent a lot or
shipment of grease softer than 175 penetration
(see Method D 217). prepare a composite sam-
ple by mixing equal portions thoroughly. Use
a large spoon or spatula in a cleaa container.
Avoid vigorous mixing or working of air into
the grease. As grease samples become partially
"worked" in being removed from containers.
the procedure is not suitable for obtaining sam-
ples of greases softer than 175 penetration on
which unworked penetration is to be deter-
mined. For greases having a penetration less
than 175. cut samples from the container with
a knife in the form of blocks about 6 by 6 by 2
in (152 by 152 by 51 mm). If required, make
unworked penetration tests on blocks as pro*
cured, and other inspection tests on grease cut
from the blocks.
10. Sampling Industrial Aromatic Hydrocar-
bons
10.1 Application—For obtaining samples of
industrial aromatic hydrocarbons (benzene, tol-
uene, xylene. and solvent naphthas), proceed in
accordance with Sections 7 to 9. particularly
those pertaining to precautions, care, and clean-
liness.
11. Samptfflf for Specific Tests
II. I Special Precautions—Special sampling
precautions and instructions are required for
some ASTM test methods and specifications.
Such instruction 11.2 to 11.3. supplement the
general procedures of this method and
supersede them if there is a conflict. ASTM
methods in this category are as follows:
ASTM Test Methods Sections
O216
D323
DS23
D>73
0261
DI8S6
D244
11.2
11.3
11.4
11.4
11.5
106
• 10.7
04057
11.2 Distillation of \aiural Gasoline—V>'hen
obtaining samples of natural gasoline that are
to be tested using Method D216. the bottle
sampling procedure. 9 1.3 is preferred. Before
obtaining the sample, precool the bottle b>
immersing it in the product, allow it to fill, and
discard the first filling. If the bottle procedure
cannot be used, obtain the sample by the tap
procedure, and with the use of the cooling bath.
as described in 9.2.3. Do not agitate the bottle
while drawing the sample. After obtaining the
sample, close the bottle immediately with a
tight-fitting stopper and store it in an ice bath
or refrigerator at a temperature of 32 to 40'F
(Oto4.5"C).
11.3 Keid yapor Pressure:
11.3.1 When sampling products that are to
be tested using Method D 323. observe the
following precautions and instructions:
11.3.1.1 Precautions—Vapor pressures are
extremely sensitive to evaporation losses and to
slight changes in composition. When obtaining.
storing, or handling samples, observe the nec-
essary precautions to ensure samples represent-
ative of the product and satisfactory for Reid
vapor pressure tests. Official samples should be
taken by. or under the immediate supervision
of. a person of judgment, skill, and sampling
experience. If sampling or sample requirements
for other tests differ from those described in
11.3.1.2 to 11.3.1.9. obtain a separate sample
for the Reid vapor pressure test. Never prepare
composite samples for this test. Make certain
that containers which are to be shipped b>
common earner conform to I.C.C.. state, or
local regulations. When flushing or purging
lines or containers, observe the penment regu-
lations and precautions against fire, explosion.
and other hazards.
11.3.1.2 Cooling Bah—A. bath (Fig. 10) of
sufficient size to hold the sample container and
a cooling cod of about 25 ft (7.6 mt of copper
tubing (*» in. (9.5 mm) or less in outside di-
ameter) shall be required when using the pro-
cedue described in 11.3.1.7 One end of the coil
is provided with a connection for attaching it
to the tank sampling tap or valve. The other
end is fitted with a suitable valve (outlet) of
good quality. A removable copper tube of l» in.
(9.5 nun) or less in outside diameter and of
sufficient length to reach the bottom of the
sample container shall be connected to the open
end of the outlet valve.
11.3.1.3 Sample Containers— Use containers
14
-------
OSWER 9951.1
of act less than I qt (0.9 L) nor more than 2-
gal (7.6-L) capacity, of sufficient strength to
withstand the pressures to which they may be
subjected, and of a type that will permit re-
placement of the cap or stopper with suitable
connections for transferring the sample to the
gasoline chamber of the vapor pressure appa-
ratus. Open-type containers have a single open-
ing which permits sampling by immersion.
Closed-type containers have two openings: one
in each end (or the equivalent thereof), fined
with valves suitable for sampling by water dis-
placement or by purging.
11.3.1.4 Transfer Connections—The transfer
connection for the open-type container consists
of an air tube and a liquid delivery tube assem-
bled in a cap or stopper. The air tube extends
to the bottom of the container. One end of the
liquid delivery tube is flush with the inside face
of the cap or stopper, and the tube is long
enough to reach the bottom of the gasoline
chamber while the sample is being transferred
to the chamber. The transfer connection for the
closed-type container consists of a single tube
with a connection suitable for attaching it to
one of the openings of the sample container.
The tube is long enough! to reach the bottom
of the gasoline chamber while the sample is
being transferred.
11.3.1.5 Sampling Open Tanks—Vie clean
containers of the open type when sampling
open tanks and tank can. An ail-level sample
obtained by the bottle procedure. 9.2.3. is rec-
ommended. Before taking the sample, flush the
container by immersing it in the product to be
sampled. Then obtain the sample immediately.
Pour off enough so that the container will be
70 to 80 % full and dose it promptly. Label the
container and. deliver it to the laboratory.
11.3.1.6 Sampling Closed Tanks—
Containers of either the open or closed type
may be used to obtain samples from closed or
prature tanks. If the open type is used, follow
the cooling bath procedure described in
11.3.1.7. If the closed type is used, obtain the
sample using the water displacement proce-
dure. 11J. 1.8, or the purging procedure.
11.3.1.9. The water displacement procedure is
preferable because the flow of product involved
in the purging procedure may be hazardous;
11.3.1.7 Cooling Bath Procedure— When us-
ing a container of the open type, keep it at a
temperature of 32 to 40'F (0 to 44°C) dunng
04OS7
the sampling operation by using the cooling
bath (Fig. 10). Connect the cod to the tank
sampling tap or valve and flush a with a suffi-
cient amount of product to ensure complete
purging. When obtaining a sample, throttle the
outlet valve so that the pressure in the coil will
be approximately the same as that in the tank.
Fill the container once to wash and cool it. and
discard the wash product. Then draw the sam-
ple immediately. Pour off enough so that the
container will be 70 to 80 % full and close it
promptly. Label the container and deliver u to
the laboratory.
11.3.1.8 Water Displacement Procedure—
Completely fill the closed-type container with
water and close the valves. The water should
be at the same temperature or lower than that
of the product to be sampled. While permitting
a small amount of product to flow through the
fitting*, connect the top or inlet valve of the
container to the tank sampling tap or valve.*
Then open all valves on the inlet side of the
container. Open the bottom or outlet valve-
slightly to allow the water to be displaced
slowly by the sample entering the container.
Regulate the flow so that there is no apprecia-
ble change in pressure within the container.
Close the outlet valve as soon as gasoline dis-
charges from the outlet: then in succession close
the' inlet valve and the sampling valve on the
tank. Disconnect the container and withdraw
enough of the contents so that it will be 70 to
80 % full If the vapor pressure of the product
is not high enough to force liquid from the
container, open both the upper and lower
valve* slightly to remove the excess. Promptly
seal and label the container, and deliver it to
the laboratory. The above is not applicable to
LPG:
11.3.1.9 forging Procedure—Connect the in-
let valve of the closed-type container to the
tank sampling tap or valve. Throttle the outlet
valve of the container so that the pressure in it
will be approximately equal to that in the con-
tainer being sampled. Allow a volume of prod-
uct equal to at least twice that of the container
to flow through the sampling system. Then
close all valves, the outlet valve first, the inlet
valve of the container second, and the tank
nmpii.ij yfjve last, and disconnect the con-
tainer immediately. Withdraw enough of the
contents so that the sample container will be
70 to 80 * full. If the vapor pressure of the
15
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OSWER 9951.1
product is oot high enough to force liquid from
the container, open both the upper and lower
valves slightly to remove the excess. Promptly
seal and label the container and deliver it to
the laboratory.
\\4OxidaitonStability.
11.41 When sampling products that are to
be tested for oxidation stability in accordance
with Method D525. Method 0873, or by
equivalent methods, observe the following pre-
cautions and instructions:
11.4.1.1 Precautions—Very small amounts
(as low as 0.001 %) of some materials, such as
inhibitors, have a considerable effect upon ox-
idation stability tests. Avoid contamination and
exposure to light while taking and handling
samples. To prevent undue agitation with air
which promotes oxidation, do not pour, shake,
or stir samples to any greater extent than nec-
essary. Never expose them to temperatures
above those necessitated by atmospheric con-
ditions.
11.4.1.2 Sample Containers—Use only
brown glass or wrapped clear glass bottles as
containers, since it is difficult to make certain
that cans are free of contaminants, such as rust
and soldering flux. Clean the bottles by the
procedure described in 9.1.3.3 and. if possible.
finish with a cleaning solution of sulfuhc acid
and potassium dichromaie. Rinse thoroughly
with distilled water, dry. and protect the bottles
from dust and din.
11.4.1.3 Sampling—An all-levels sample ob-
tained by the bottle procedure. 9.2.3.1. is rec-
ommended because the sample is taken directly
in the bottle. This reduces the possibility of air
absorption, loss of vapors, and contamination.
Just before sampling, rinse the bottle with the
gasoline to be sampled.
11.5 Lacquer'Solvents and Diluentr.
11.5.1 When sampling bulk shipments of
lacquer solvents and diluents that are to be
tested using Method D 268. observe the follow-
ing precautions and instructions:
11.5.1.1 Tanks and Tank Can—Obtain up-
per and lower samples (Fig. I) of not more than
040S7
1 qt at (0.9 L) each by the bottle procedure.
9.2.3.2. Prepare in the laboratory' a composite
sample of not less than '-. gal < 1.9 Li by mixing
equal pans of the upper and lower samples.
11.5.1.2 Barrels. Drums, and Cans—Obtain
samples from at least five percent of the number
of containers in any shipment. The number of
containers to be sampled may be increased at
the discretion of the purchaser. In the case- of
expensive solvents which are purchased in
small quantities, it is recommended that each
container be sampled. Withdraw a portion
from the center of each container to be sampled
with a clean tube (9.6.3) or weighted bottle
(9.2.3.2). (A smaller bottle may be used.) Pre-
pare a composite sample of at least I qt (0.93
L) by mixing equal portions of not less than I
pt (0.47 L) from each container sampled.
\\.6Asphaitic Materials—When sampling
asphaltic materials that are to be tested using
Method O 1856 or Method 0 2171 obtain sam-
ples by the boring procedure (9.8.3) or the grab
procedure (9.8.3). A sample of sufficient sue to
yield at least 100 g of recovered bitumen is
required. About 1000 g of sheet-asphalt mix-
tures usually will be sufficient. If the largest
lumps in the sample are I in. (25.4 mm). 2000
g will usually be required, and still larger sam-
ples if the mixtures contain larger aggregates.
11.7 Emulsified Asphalts—\\ is frequently
necessary to test samples in accordance with
the requirements of Specifications O *7~. and
Method D 244. Obtain samples from tanks.
tank cars, and tank trucks by the bottle sam-
pling procedure. 9 2.3. using a wide-mouth 11L.-
in. (38.t-mm)or greater* bottle. Use the dipper
procedure. 9.5.3. to obtain samples from filling
or discharge lines. Sample packages in accord-
ance with Table 3. If the material is solid or
semisolid. use the bonng sampling procedure.
9.8.4. Obtain at least I gal (13.8 L) or 10 Ib (4.5
kg) from each lot or shipment. Store the sam-
ples in clean, airtight containers at a tempera-
ture of not less than 4aC until tested. Use glass
or black iron containers for emulsified asphalts
of the RS-I type.
16
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OSWER 9951.1
4 04037
T48LE I Summary of Stratum Procedure* and
Application
Type 01' Container
Procedure
Liquids of mor> than 16 p»i (110
tP»i aad aoi more (baa 26 pu
Liquid* of mar* (ban 16 pu 1 1 10
kPn and not mort tbao 26 pa
(|79kPa>Rvp
Liquid! of mort than 1 pu ( M.I kPat
aod on nor* loan 16 pa < 1 10 kpai
Rvp
Liquid! of mort than 2 asi (1)1 kPal
and ooi montbaa Iapu
Rvp
Liquids of 16 pu 1 1 10 kPi) of leu
Rvp
Liquids of 2 pu (131 kPa) or lev
R.p
Liquid! of 2 pu (13.1 kPt) or leu
Rvp
Liquids of 2 pu (13.1 kPa) or leu
Rvp
Liquids of 2 p*i (131 kfii or less-
R.p
Boiiom or ibitf sampling of liquids
of 2 psi(l) S kPti Rvp or leu
Uquidi and MiiiUiqiudiof 2 pu 1 1 3.1
kPai Rvp or Leu
Crude petroleum
Industrial aromatic bydracarbons
Waxes, solid bitumens, and other
sort solids
Petroleum coke: lumpy souda,
Creases, soft waxes, asphalt*
Aspbaltic matenals
Emulsified aspbalu
siora;r taaki. ibip and barge tanu. tank can.
lank trudu
storage taakJ *na up*
storage tank*, ship and barge tank*, tank can.
tank trucks
storage tank* with taps
pipe* or lines
storage tanks, ship and barge
storage tanks with taps
fret or open-discharge streams
drums, barrels, and cans
tank can. storage tanks
free or operi-discharfc streams. Open tanks or
kettles »n1 open Beads: tank can and taak
trucks: drums
storage tanks, ship and barge tank*, tank can.
tank truck*, aad pipelines
storage tanks, ship and barge tanks
barrels, cases, bags, cakes
freight can. conveyon. bags, barrels, boxes
kettles drums, cans, tubes
storage tanks, tank can. unes. packages
storage tanks, tana can. lines. r-vHigf*
precooled bottle sampling
cooler tap sampling
bottle sampling
tap sampling
IB-
bc*U« sampling
tap sampling
dipper sampling
tube sampling
thief sampling
dipper sampling
automatic sampling thief
sampling bottle sampling
tap sampling
bottle sampling
bonng sampling
grab sampling
grease sampling
TABLE 2
l»«rmHe«i for H
Crtaekfeal Taaks
TABLE!
Liquid
Depth. *
Diameter
Sampling Level
* of Diameter
Abov«Botioea
Composite Sample.
Proportionate Parts
•
Upper/ MMtdle/ Lower 1 Upper/ Middle/ Lower
100 SO
90 i 75
SO
70
tt
*"J§»'
i^jjgfc
JiXfr.
!••»•
!t?*?
70
50-
50
50
50
50
40
20
20
20
20
20
20
20
15
10
5
3
3
2
4
4
5
6
5
4
3
3
3
4
5
6
: ' 10
I
1
10
10
10
Nmtber of Pwtafti t« be Setoctrt
forSaeapttMj
Number of
Packages in Lot
1 to 3
41064
65 to 125
126 to 216
217 to 343
344to5l2
5 13 to 7:9
730 10 1000
lOOlu 1331
Number
of Pack-
ages to
Be Sam-
pled
all
4
5
6
7
S
9
10
II
Number of
Packages in Lot
1332 to 1778
1729 to 2 197
2l9Su>2744
2745 to J375
3376 to 409ft
4097(04913
49l4to5832
5S33 to 6S59
6MOorover
Number
pled
12
13
14
15
16
17
19
:o
17
-------
OSWER 9951.1
fP 04057
TABLE 4 WMftoe* S«e**ii« Bottte <
NOTI—See running or aU-leveli uoipiei (» 2.3)
Oumctcr
Material of Op«a-
Light lubricating oil*, kerouae*. gae>
olines. tnniptmt gat oib. dMMl
fuel*, tod duiitUiM
Hejvv lubncauag oU*. oocmjuo*/-
caigMoilf
Lgii erode oil* (leu ihafl 2001 Say.
bolt L'aivenaJ Vitcouiyai IQO'F)
Heaw crude aad fuel oil*
(19)
(3D
(19)
no
TAILE 5 SbtrfCr**M
Mtainun Sample
Tuba or fMCktga. lew ilua I 16
l-lbcui
5 or 10-lbciM
Larger i6»fl lOlb
UrgtrtAtf 10 Ib
UrgcrtbM 10 Ib
eoougb uaiu for * Mb uapit
ail
leu tiun 10 000 Ib
10 00010 JO 000 Ib
oor«bM50 000 Ik
OMCM
2 u> 3 Ib from OM or more eooutacn
2 u> i Ib (ram rwo or osort coautacn
2 10 5 Ib-frew ttnt or more coouioen
HATCH
.«"
.-y. TOP SAMPLE
« U^HfJSAMnC
• MIDDLE SAMPLE
3. 1 IOWCR SAMPLE
5 CLEARANCE SAKPLE
UPfCM TMIIO
MIMLE THIRD
LOWER THIRD
•WTTOM SAMPLE
Han— Tht eoclM u«pt* lo
fro* ib« floor of IJM tut or tunu dova into a wap.
FIC. I
i only to d« outlca. It don oot apprr wbea (be ouilei comn
18
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OSWER 9951.1
0 4057
'/•"COPPER
WIRE—
HANDLE
(•) l-Ot Weightfd Boula
(»l I-O
FIG. 2
1 Qt Weighted Beaker
19
-------
OSWER 9951.1
0 4057
TAIMK
FIG. J
• ttVCL
( A)
I /••-!/«• »I»C
TO MCCIVCN
on
'»!'
Oi
CNO «CAMCO ro
A SHAH* fOOf
omricc IN Sioi of fmout
•«O«C re tl CL04CD
ro •cecivcH
on SAM»LC*
< • > C C I
I< >••• «r « »irrt» •»• v.x* M *VM •
FIG. 4 Pro6n for Coaiiauon* S«apiiB|
20
-------
OSWER 9951.1
04057
FTC. 5
21
-------
OSWER 9951.1
04097
-U
— 11
-10
— 7
F1C. «
PC. T
22
-------
OSWER 9951.1
04057
1. i UNtrN Of CM •
'1
•—
oo
oo
4T!I
i?. SI
—»- «
FIG. I Uc«tM^SMpta«f«MiMOM |