1、Designation: D7482 15D7482 17Standard Practice forSampling, Storage, and Handling of Hydrocarbons forMercury Analysis1This standard is issued under the fixed designation D7482; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This practice covers the types of and preparation of containers found most suitable for the handling of hydroca
3、rbon samplesfor 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 mixtureof dissolved Hg(0) atoms, adsorbed Hg(0) on particulates (for example, carbonaceous or mineral fines and Fe2O3) and suspende
4、ddroplets of metallic mercury.1.3 The presence of suspended droplets of metallic mercury (often called “colloidal” mercury, since the droplet size can be verysmall) can make obtaining a representative sample very difficult for a variety of reasons (for example, non-isokinetic sampling ofthe liquid c
5、an result in over- or under-collection of suspended droplets and collection of mercury that has accumulated in denselarger drops and pools on the bottom of piping and in sample taps). Pay strict attention to the detailed procedure (Section 7) toensure representative samples are collected.1.4 When re
6、presentative test portions are collected and analyzed in accordance with acceptable procedures, the total mercuryis 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
7、Mercury has been designated by EPA and many state agencies as a hazardous material that can cause centralnervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury-containing product
8、s. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs website (http:/www.epa.gov/mercury/faq.htm) for additional information. Users should be awarethat selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.1.7 This standar
9、d does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.8 This international standard w
10、as developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced
11、 Documents2.1 ASTM Standards:2D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and LubricantsD7622 Test Method for Total Mercury in Crude Oil Using Combustion and Direct Cold Vapor Atomic Absorption Method withZeeman Background CorrectionD7623 Test Method for Total Mercury in Crude Oi
12、l Using Combustion-GoldAmalgamation and Cold VaporAtomicAbsorptionMethod2.2 EPA Standard:3EPA Method 1669 Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels; July 1996; USEnvironmental Protection Agency1 This practice is under the jurisdiction of ASTM Committee D02 on Petro
13、leum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved Nov. 1, 2015July 1, 2017. Published November 2015July 2017. Originally approved in 2008. Last previous edition approved in 20142015 asD7482 14.D7482 15. D
14、OI: 10.1520/D7482-15.10.1520/D7482-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from United
15、 States Environmental Protection Agency (EPA), Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460 (www.epa.gov).This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Bec
16、auseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appe
17、ars at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsFor definitions of terms used in this standard, refer to Terminology D4175.3.2 Abbreviations:3.2.1 VOAVolatile Organic Analysi
18、s4. Summary of Practice4.1 This practice describes the sampling, storage, transport, and handling of hydrocarbon samples used for determining mercury,and the precautions that need to be taken to prevent sample contamination and loss of analyte.5. Significance and Use5.1 This practice is intended for
19、 use in sampling liquid hydrocarbons including crude oils, condensates, refinery processintermediates, and refined products. Generally these samples are expected to contain mercury from the parts per billion (10-99mass) to parts per million (10-66 mass) range.5.2 This practice is not intended for us
20、e when sampling aqueous systems where the concentrations of mercury are often in theparts per trillion (10-1212 mass) range. These samples are often better addressed by using the rigorously clean techniques from theEPA Method 1669 “clean hands, dirty hands” sampling procedures.5.3 This practice is n
21、ot intended for use for liquefied samples, for which special containers may be required for pressurizedsamples.5.4 This practice is only suitable for stabilized samples which remain 100 % liquid at ambient conditions. For samples that ondepressurization lose some of the light hydrocarbon ends it is
22、important to note that elemental mercury may be lost duringsampling. Sampling modules which inject unstabilized liquid hydrocarbons close to process conditions directly to the mercuryanalyzer can be used to overcome this issue.5.5 Based on this practice, two Test Methods (D7622 and D7623) are availa
23、ble for determination of mercury in crude oil, basedon 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 maycondense water as the sample cools from process temperature to ambient temperature. Ion
24、ic mercury species are water soluble andthese 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 hygieneconcern.6. Apparatus6.1 Clear or Amber Borosilicate Glass, 40 mL
25、 or less in volume; pre-cleaned by acid-washing; with PTFE(polytetrafluoroethylene)-lined septum caps. These are commonly referred to as VOA vials and are used for many water samplesusing EPA methods.6.1.1 The use of 30 mLor smaller VOAvials may allow shipment of multiple sample vials as “excepted q
26、uantities” under IATA(International Air Transport Association) regulations. Determine specific shipping requirements with the appropriate knowledge-able personnel.6.2 Alternate ContainersQuartz. Epoxy-lined, tin-lined, or steel cans for direct or sub-sample may not be acceptable because,in some case
27、s, these types of containers show a significant depletion of mercury (see 9.1 and 9.2).6.2.1 Tin-lined steel cans, direct or sub-sample, are not acceptable.6.3 Chain of Custody Forms.6.4 Permanent Marking Pens.6.5 Resealable BagsClear, plastic, 1 L capacity.7. Sampling Procedure7.1 Employ the normal
28、 hydrocarbon sampling procedures necessary to obtain discrete and homogeneous samples. Either grabsamples or composites from auto-samplers are allowed. Grab samples are preferred. When expecting particulates with adsorbedmercury or mercury droplets, iso-kinetic sampling is greatly preferred.7.2 Wash
29、 the VOA vials with nitric acid, rinse with water, and dry.7.3 A sample “set” is defined as three VOA glass vials. Each vial is individually wrapped with a plastic bag, and then the setof three vials are overpacked in an appropriate container for transport or shipping. A set of three individually ba
30、gged sample vialsmay be bundled together and placed in a larger bag to separate them from other sample sets included in the same shipment.Adsorbant material may be packed around the bagged vials to further protect against damage during shipping and release of oneor more of the sample vials if it rup
31、tures.D7482 1727.4 One sample set is required for each sampling event. Fill three sample vials for each oil sampled as close to the same pointin time as possible.7.5 Sampling shall be done directly into the VOA vials if possible. If it is necessary to sample into one container and thentransfer into
32、the VOA vial, record the details of the original container and sampling method, as well as the details of the transfer.Auto-samplers are acceptable, but the container and plumbing materials and transfer details shall be documented in the notebookor Chain of Custody (COC) form.7.6 Purge sample taps s
33、ufficiently immediately prior to sampling to remove any elemental mercury droplets that haveaccumulated in the piping, valve, or crevices. In some cases, significant amounts of elemental mercury have been found toaccumulate in sample taps. Proper collection or recycling of the purge is important to
34、prevent release of mercury and workerexposure.7.7 It is imperative that persons conducting or supervising the sampling procedure understand the conditions that causeevaporative or other loss of mercury. While bulk mercury droplets are not highly volatile (vapor pressure 1 L).10. Analysis of Crude Oi
35、l10.1 Two methods for determination of mercury in crude oil are described in Test Methods D7622 and D7623, both based onelectrothermal volatilization of mercury species and subsequent atomic spectroscopic determination.10.2 Repeatability of analysis of these analyses in the 5 ng HgmL to 400 ng Hg/mL
36、 given in these standards is as follows:D7622 0.7147 X0.60D7623 0.4396 X0.5864Where X is the average mercury concentration in ng/mL.10.3 Reproducibility of the analyses has not been determined. Volatility of mercury compounds and elemental mercury presentin crude oil has been documented elsewhere.4
37、Further, replicate laboratory analyses on the same sample have found decreases inmercury concentration over time.5 Also, see the discussion about mercury occurrence in crude oils above in 1.2 and 1.3. Becauseof this, it is not practical to distribute the crude oil samples to laboratories and get rep
38、roducible results. Hence, the reproducibilityof this these test methods is not expected to be determined in the near future.11. Pollution Prevention and Waste Management11.1 Draw samples in accordance with both the facility requirements and applicable laws and regulations.Appropriate personalprotect
39、ive equipment shall be worn at all times. Return purge streams directly to the process, or collect for disposal or recycling.11.2 Free elemental mercury, collected as a separate material or contained with the hydrocarbon sample, shall be treated withextreme caution. Personal exposure to vapors from
40、free mercury droplets or puddles can exceed exposure limits. Appropriatepersonal protective equipment shall be worn by the sampling team whenever exposure is possible.4 Giles, H. N. and Mills, C. O., “Crude Oils: Their Sampling, Analysis, and Evaluation,” ASTM International Press, West Conshohocken,
41、 PA, Manual 68, 2010.5 Wilhelm, S. M., Kirchgessner, D. A., Liang, L., and Kariher, P. H., “Sampling and Analysis of Mercury in Crude Oil,” STP 1468, Elemental Analysis of Fuels andLubricants: Recent Advances and Future Prospects, Nadkarni, R. A., Ed., ASTM International Press, West Conshohocken, PA
42、, 2005.D7482 17411.3 Elemental mercury can be collected (for example, using a mercury vacuum) for disposal, or rendered less hazardous bytreating with various sulfur compounds or finely dispersed metal powders (for example, zinc, when activated by mild acid wash)to convert it to less-volatile and le
43、ss toxic compounds. Facility procedures for responding to releases of elemental mercury shallbe applied.11.4 Disposal of mercury-contaminated materials, elemental mercury, or mercury compounds shall be referred to the facilityhazardous waste coordinator.12. Keywords12.1 handling; mercury; mercury an
44、alysis; sampling; storageBIBLIOGRAPHY(1) Bloom, N. S., Fresenius Journal of Analytical Chemistry, Vol 366, 2000, pp. 438-443.443.(2) Wilhelm, S. M., Kirchgessner, D. A., Liang, L., and Kariher, P. H., “Sampling and Analysis of Mercury in Crude Oil,” Elemental Analysis of Fuelsand Lubricants: Recent
45、Advances and Future Prospects, Nadkarni, R. A. Kishore, editor, STP1468, ASTM International, 2005, p. 183.SUMMARY OF CHANGESSubcommittee D02.03 has identified the location of selected changes to this standard since the last issue(D7482 14D7482 15) that may impact the use of this standard. (Approved
46、Nov. 1, 2015.)July 1, 2017.)(1) Added Test Methods D7622 and D7623 to Referenced Documents.(1) Added information about these added standards in the new subsectionInformation on the precision of two standard test methodsfor mercury determination has been added in a new Section 5.510.Subcommittee D02.
47、03 has identified the location of selected changes to this standard since the last issue(D7482 08) that may impact the use of this standard. (Approved Oct. 1, 2014.)(1) Added new sections 5.4, 5.6, and 8.2.5 to include information on stability of mercury samples.ASTM International takes no position
48、respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.Th
49、is standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee
