ASTM D7482-17(2023)
(Practice)Standard Practice for Sampling, Storage, and Handling of Hydrocarbons for Mercury Analysis
Standard Practice for Sampling, Storage, and Handling of Hydrocarbons for Mercury Analysis
SIGNIFICANCE AND USE
5.1 This practice is intended for use in sampling liquid hydrocarbons including crude oils, condensates, refinery process intermediates, and refined products. Generally these samples are expected to contain mercury from the parts per billion (10–9 mass) to parts per million (10–6 mass) range.
5.2 This practice is not intended for use when sampling aqueous systems where the concentrations of mercury are often in the parts per trillion (10–12 mass) range. These samples are often better addressed by using the rigorously clean techniques from the EPA Method 1669 “clean hands, dirty hands” sampling procedures.
5.3 This practice is not intended for use for liquefied samples, for which special containers may be required for pressurized samples.
5.4 This practice is only suitable for stabilized samples which remain 100 % liquid at ambient conditions. For samples that on depressurization lose some of the light hydrocarbon ends it is important to note that elemental mercury may be lost during sampling. Sampling modules which inject unstabilized liquid hydrocarbons close to process conditions directly to the mercury analyzer can be used to overcome this issue.
5.5 Based on this practice, two Test Methods (D7622 and D7623) are available for determination of mercury in crude oil, based on cold vapor atomic absorption technique.
5.6 In some refined streams and in tank samples free water may be present. Process streams that are water saturated may condense water as the sample cools from process temperature to ambient temperature. Ionic mercury species are water soluble and these water droplets may contain mercury or adsorb mercury over time.
5.7 The presence of mercury during crude oil production, transport, and refining can be an environmental and industrial hygiene concern.
SCOPE
1.1 This practice covers the types of and preparation of containers found most suitable for the handling of hydrocarbon samples for the determination of total mercury.
1.2 This practice was developed for sampling streams where the mercury speciation is predominantly Hg(0) present as a mixture of dissolved Hg(0) atoms, adsorbed Hg(0) on particulates (for example, carbonaceous or mineral fines and Fe2O3) and suspended droplets of metallic mercury.
1.3 The presence of suspended droplets of metallic mercury (often called “colloidal” mercury, since the droplet size can be very small) can make obtaining a representative sample very difficult for a variety of reasons (for example, non-isokinetic sampling of the liquid can result in over- or under-collection of suspended droplets and collection of mercury that has accumulated in dense larger drops and pools on the bottom of piping and in sample taps). Pay strict attention to the detailed procedure (Section 7) to ensure representative samples are collected.
1.4 When representative test portions are collected and analyzed in accordance with acceptable procedures, the total mercury is representative of concentrations in the sample.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and envi...
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7482 − 17 (Reapproved 2023)
Standard Practice for
Sampling, Storage, and Handling of Hydrocarbons for
Mercury Analysis
This standard is issued under the fixed designation D7482; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope tion. Users should be aware that selling mercury or mercury-
containing products, or both, in your state may be prohibited by
1.1 This practice covers the types of and preparation of
state law.
containers found most suitable for the handling of hydrocarbon
1.7 This standard does not purport to address all of the
samples for the determination of total mercury.
safety concerns, if any, associated with its use. It is the
1.2 This practice was developed for sampling streams where
responsibility of the user of this standard to establish appro-
the mercury speciation is predominantly Hg(0) present as a
priate safety, health, and environmental practices and deter-
mixture of dissolved Hg(0) atoms, adsorbed Hg(0) on particu-
mine the applicability of regulatory limitations prior to use.
lates (for example, carbonaceous or mineral fines and Fe O )
2 3
1.8 This international standard was developed in accor-
and suspended droplets of metallic mercury.
dance with internationally recognized principles on standard-
1.3 The presence of suspended droplets of metallic mercury ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
(often called “colloidal” mercury, since the droplet size can be
very small) can make obtaining a representative sample very mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
difficult for a variety of reasons (for example, non-isokinetic
sampling of the liquid can result in over- or under-collection of
2. Referenced Documents
suspended droplets and collection of mercury that has accu-
mulated in dense larger drops and pools on the bottom of 2.1 ASTM Standards:
piping and in sample taps). Pay strict attention to the detailed D4175 Terminology Relating to Petroleum Products, Liquid
procedure (Section 7) to ensure representative samples are Fuels, and Lubricants
collected. D7622 Test Method for Total Mercury in Crude Oil Using
Combustion and Direct Cold Vapor Atomic Absorption
1.4 When representative test portions are collected and
Method with Zeeman Background Correction
analyzed in accordance with acceptable procedures, the total
D7623 Test Method for Total Mercury in Crude Oil Using
mercury is representative of concentrations in the sample.
Combustion-Gold Amalgamation and Cold Vapor Atomic
1.5 The values stated in SI units are to be regarded as
Absorption Method
standard. No other units of measurement are included in this
2.2 EPA Standard:
standard.
EPA Method 1669 Sampling Ambient Water for Trace Met-
als at EPA Water Quality Criteria Levels; July 1996; US
1.6 Warning—Mercury has been designated by EPA and
Environmental Protection Agency
many state agencies as a hazardous material that can cause
central nervous system, kidney, and liver damage. Mercury, or
3. Terminology
its vapor, may be hazardous to health and corrosive to
3.1 Definitions—For definitions of terms used in this
materials. Caution should be taken when handling mercury and
standard, refer to Terminology D4175.
mercury-containing products. See the applicable product Ma-
terial Safety Data Sheet (MSDS) for details and EPA’s website
3.2 Abbreviations:
(http://www.epa.gov/mercury/faq.htm) for additional informa-
3.2.1 VOA—Volatile Organic Analysis
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- Standards volume information, refer to the standard’s Document Summary page on
mittee D02.03 on Elemental Analysis. the ASTM website.
Current edition approved July 1, 2023. Published July 2023. Originally approved Available from United States Environmental Protection Agency (EPA), Ariel
in 2008. Last previous edition approved in 2017 as D7482 – 17. DOI: 10.1520/ Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460 (www.epa.gov).
D7482-17R23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7482 − 17 (2023)
4. Summary of Practice 6.2.1 Tin-lined steel cans, direct or sub-sample, are not
acceptable.
4.1 This practice describes the sampling, storage, transport,
and handling of hydrocarbon samples used for determining 6.3 Chain of Custody Forms.
mercury, and the precautions that need to be taken to prevent
6.4 Permanent Marking Pens.
sample contamination and loss of analyte.
6.5 Resealable Bags—Clear, plastic, 1 L capacity.
5. Significance and Use
7. Sampling Procedure
5.1 This practice is intended for use in sampling liquid
hydrocarbons including crude oils, condensates, refinery pro- 7.1 Employ the normal hydrocarbon sampling procedures
cess intermediates, and refined products. Generally these necessary to obtain discrete and homogeneous samples. Either
samples are expected to contain mercury from the parts per
grab samples or composites from auto-samplers are allowed.
–9 –6
billion (10 mass) to parts per million (10 mass) range. Grab samples are preferred. When expecting particulates with
adsorbed mercury or mercury droplets, iso-kinetic sampling is
5.2 This practice is not intended for use when sampling
greatly preferred.
aqueous systems where the concentrations of mercury are often
–12
in the parts per trillion (10 mass) range. These samples are
7.2 Wash the VOA vials with nitric acid, rinse with water,
often better addressed by using the rigorously clean techniques and dry.
from the EPA Method 1669 “clean hands, dirty hands” sam-
7.3 A sample “set” is defined as three VOA glass vials. Each
pling procedures.
vial is individually wrapped with a plastic bag, and then the set
5.3 This practice is not intended for use for liquefied
of three vials are overpacked in an appropriate container for
samples, for which special containers may be required for transport or shipping. A set of three individually bagged sample
pressurized samples. vials may be bundled together and placed in a larger bag to
separate them from other sample sets included in the same
5.4 This practice is only suitable for stabilized samples
shipment. Adsorbant material may be packed around the
which remain 100 % liquid at ambient conditions. For samples
bagged vials to further protect against damage during shipping
that on depressurization lose some of the light hydrocarbon
and release of one or more of the sample vials if it ruptures.
ends it is important to note that elemental mercury may be lost
during sampling. Sampling modules which inject unstabilized 7.4 One sample set is required for each sampling event. Fill
liquid hydrocarbons close to process conditions directly to the three sample vials for each oil sampled as close to the same
mercury analyzer can be used to overcome this issue. point in time as possible.
5.5 Based on this practice, two Test Methods (D7622 and 7.5 Sampling shall be done directly into the VOA vials if
D7623) are available for determination of mercury in crude oil,
possible. If it is necessary to sample into one container and
based on cold vapor atomic absorption technique. then transfer into the VOA vial, record the details of the
original container and sampling method, as well as the details
5.6 In some refined streams and in tank samples free water
of the transfer. Auto-samplers are acceptable, but the container
may be present. Process streams that are water saturated may
and plumbing materials and transfer details shall be docu-
condense water as the sample cools from process temperature
mented in the notebook or Chain of Custody (COC) form.
to ambient temperature. Ionic mercury species are water
soluble and these water droplets may contain mercury or
7.6 Purge sample taps sufficiently immediately prior to
adsorb mercury over time. sampling to remove any elemental mercury droplets that have
accumulated in the piping, valve, or crevices. In some cases,
5.7 The presence of mercury during crude oil production,
significant amounts of elemental mercury have been found to
transport, and refining can be an environmental and industrial
accumulate in sample taps. Proper collection or recycling of
hygiene concern.
the purge is important to prevent release of mercury and
worker exposure.
6. Apparatus
6.1 Clear or Amber Borosilicate Glass, 40 mL or less in 7.7 It is imperative that persons conducting or supervising
volume; pre-cleaned by acid-washing; with PTFE the sampling procedure understand the conditions that cause
(polytetrafluoroethylene)-lined septum caps. These are com- evaporative or other loss of mercury. While bulk mercury
monly referred to as VOA vials and are used for many water droplets are not highly volatile (vapor pressure <1 mmHg at
samples using EPA methods. 20 °C) in many hydrocarbons, the dissolved mercury readily
6.1.1 The use of 30 mL or smaller VOA vials may allow evaporates with an apparent vapor pressure similar to butane or
shipment of multiple sample vials as “excepted quantities” pentane. Also, mercury can readily adsorb on many metal
under IATA (International Air Transport Association) regula- surfaces. Sample taps shall not contain process-contact mate-
tions. Determine specific shipping requirements with the ap- rials composed of copper, zinc, tin, aluminum, brass, bronze,
propriate knowledgeable personnel. Monel or other alloys containing these metals.
6.2 Alternate Containers—Quartz. Epoxy-lined, tin-lined, 7.8 To avoid loss of mercury vapor from the samples,
or steel cans for direct or sub-sample may not be acceptable proceed as follows:
because, in some cases, these types of containers show a 7.8.1 Fill the vial as quickly as possible, filling
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