1、Designation: D7482 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 year of la
2、st 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 ofcontainers found most suitable for the handling of hydrocarbonsampl
3、es for the determination of total mercury.1.2 This practice was developed for sampling streams wherethe mercury speciation is predominantly Hg(0) present as amixture of dissolved Hg(0) atoms, adsorbed Hg(0) on particu-lates (for example, carbonaceous or mineral fines and Fe2O3)and suspended droplets
4、 of metallic mercury.1.3 The presence of suspended droplets of metallic mercury(often called “colloidal” mercury, since the droplet size can bevery small) can make obtaining a representative sample verydifficult for a variety of reasons (for example, non-isokineticsampling of the liquid can result i
5、n over- or under-collection ofsuspended droplets and collection of mercury that has accu-mulated in dense larger drops and pools on the bottom ofpiping and in sample taps). Pay strict attention to the detailedprocedure (Section 7) to ensure representative samples arecollected.1.4 When representative
6、 test portions are collected andanalyzed in accordance with acceptable procedures, the totalmercury is representative of concentrations in the sample.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 WarningMercury has bee
7、n designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney, and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury-containing products. See the applica
8、ble product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for additional informa-tion. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited bystate law.1.7 This standard does not purpo
9、rt to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.8 This international standard was developed i
10、n accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2
11、.1 ASTM Standards:2D4175 Terminology Relating to Petroleum Products, LiquidFuels, and LubricantsD7622 Test Method for Total Mercury in Crude Oil UsingCombustion and Direct Cold Vapor Atomic AbsorptionMethod with Zeeman Background CorrectionD7623 Test Method for Total Mercury in Crude Oil UsingCombus
12、tion-Gold Amalgamation and Cold Vapor AtomicAbsorption Method2.2 EPA Standard:3EPA Method 1669 Sampling Ambient Water for Trace Met-als at EPA Water Quality Criteria Levels; July 1996; USEnvironmental Protection Agency3. Terminology3.1 DefinitionsFor definitions of terms used in thisstandard, refer
13、to Terminology D4175.3.2 Abbreviations:3.2.1 VOAVolatile Organic Analysis1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.03 on Elemental Analysis.Current edition approved July 1, 2
14、017. Published July 2017. Originally approvedin 2008. Last previous edition approved in 2015 as D7482 15. DOI: 10.1520/D7482-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informatio
15、n, refer to the standards Document Summary page onthe ASTM website.3Available from United States Environmental Protection Agency (EPA), ArielRios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460 (www.epa.gov).*A Summary of Changes section appears at the end of this standardThis international
16、standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14
17、. Summary of Practice4.1 This practice describes the sampling, storage, transport,and handling of hydrocarbon samples used for determiningmercury, and the precautions that need to be taken to preventsample contamination and loss of analyte.5. Significance and Use5.1 This practice is intended for use
18、 in sampling liquidhydrocarbons including crude oils, condensates, refinery pro-cess intermediates, and refined products. Generally thesesamples are expected to contain mercury from the parts perbillion (109mass) to parts per million (106mass) range.5.2 This practice is not intended for use when sam
19、plingaqueous systems where the concentrations of mercury are oftenin the parts per trillion (1012mass) range. These samples areoften better addressed by using the rigorously clean techniquesfrom the EPA Method 1669 “clean hands, dirty hands” sam-pling procedures.5.3 This practice is not intended for
20、 use for liquefiedsamples, for which special containers may be required forpressurized samples.5.4 This practice is only suitable for stabilized sampleswhich remain 100 % liquid at ambient conditions. For samplesthat on depressurization lose some of the light hydrocarbonends it is important to note
21、that elemental mercury may be lostduring sampling. Sampling modules which inject unstabilizedliquid hydrocarbons close to process conditions directly to themercury analyzer can be used to overcome this issue.5.5 Based on this practice, two Test Methods (D7622 andD7623) are available for determinatio
22、n of mercury in crude oil,based on cold vapor atomic absorption technique.5.6 In some refined streams and in tank samples free watermay be present. Process streams that are water saturated maycondense water as the sample cools from process temperatureto ambient temperature. Ionic mercury species are
23、 watersoluble and these water droplets may contain mercury oradsorb mercury over time.5.7 The presence of mercury during crude oil production,transport, and refining can be an environmental and industrialhygiene concern.6. Apparatus6.1 Clear or Amber Borosilicate Glass, 40 mL or less involume; pre-c
24、leaned by acid-washing; with PTFE(polytetrafluoroethylene)-lined septum caps. These are com-monly referred to as VOA vials and are used for many watersamples using EPA methods.6.1.1 The use of 30 mL or smaller VOA vials may allowshipment of multiple sample vials as “excepted quantities”under IATA (I
25、nternational Air Transport Association) regula-tions. Determine specific shipping requirements with the ap-propriate knowledgeable personnel.6.2 Alternate ContainersQuartz. Epoxy-lined, tin-lined,or steel cans for direct or sub-sample may not be acceptablebecause, in some cases, these types of conta
26、iners show asignificant depletion of mercury (see 9.1 and 9.2).6.2.1 Tin-lined steel cans, direct or sub-sample, are notacceptable.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 hydrocarbon sampling pro
27、ceduresnecessary to obtain discrete and homogeneous samples. Eithergrab samples or composites from auto-samplers are allowed.Grab samples are preferred. When expecting particulates withadsorbed mercury or mercury droplets, iso-kinetic sampling isgreatly preferred.7.2 Wash the VOA vials with nitric a
28、cid, rinse with water,and dry.7.3 Asample “set” is defined as three VOAglass vials. Eachvial is individually wrapped with a plastic bag, and then the setof three vials are overpacked in an appropriate container fortransport or shipping.Aset of three individually bagged samplevials may be bundled tog
29、ether and placed in a larger bag toseparate them from other sample sets included in the sameshipment. Adsorbant material may be packed around thebagged vials to further protect against damage during shippingand release of one or more of the sample vials if it ruptures.7.4 One sample set is required
30、for each sampling event. Fillthree sample vials for each oil sampled as close to the samepoint in time as possible.7.5 Sampling shall be done directly into the VOA vials ifpossible. If it is necessary to sample into one container andthen transfer into the VOA vial, record the details of theoriginal
31、container and sampling method, as well as the detailsof the transfer. Auto-samplers are acceptable, but the containerand plumbing materials and transfer details shall be docu-mented in the notebook or Chain of Custody (COC) form.7.6 Purge sample taps sufficiently immediately prior tosampling to remo
32、ve 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 ofthe purge is important to prevent release of mercury andworker exposure.7.7 I
33、t is imperative that persons conducting or supervisingthe sampling procedure understand the conditions that causeevaporative or other loss of mercury. While bulk mercurydroplets are not highly volatile (vapor pressure 1 L).10. Analysis of Crude Oil10.1 Two methods for determination of mercury in cru
34、de oilare described in Test Methods D7622 and D7623, both basedon electrothermal volatilization of mercury species and subse-quent atomic spectroscopic determination.10.2 Repeatability of analysis of these analyses in the5 ng Hg mL to 400 ng Hg/mL given in these standards is asfollows:D7622 0.7147 X
35、0.60D7623 0.4396 X0.5864Where X is the average mercury concentration in ng/mL.10.3 Reproducibility of the analyses has not been deter-mined. Volatility of mercury compounds and elemental mer-cury present in crude oil has been documented elsewhere.4Further, replicate laboratory analyses on the same s
36、ample havefound decreases in mercury concentration over time.5Also, seethe discussion about mercury occurrence in crude oils above in1.2 and 1.3. Because of this, it is not practical to distribute thecrude oil samples to laboratories and get reproducible results.Hence, the reproducibility of this th
37、ese test methods is notexpected to be determined in the near future.11. Pollution Prevention and Waste Management11.1 Draw samples in accordance with both the facilityrequirements and applicable laws and regulations. Appropriatepersonal protective equipment shall be worn at all times.Return purge st
38、reams directly to the process, or collect fordisposal or recycling.11.2 Free elemental mercury, collected as a separate mate-rial or contained with the hydrocarbon sample, shall be treatedwith extreme caution. Personal exposure to vapors from freemercury droplets or puddles can exceed exposure limit
39、s.Appropriate personal protective equipment shall be worn bythe sampling team whenever exposure is possible.11.3 Elemental mercury can be collected (for example,using a mercury vacuum) for disposal, or rendered lesshazardous by treating with various sulfur compounds or finelydispersed metal powders
40、(for example, zinc, when activated bymild acid wash) to convert it to less-volatile and less toxiccompounds. Facility procedures for responding to releases ofelemental mercury shall be applied.11.4 Disposal of mercury-contaminated materials, elemen-tal mercury, or mercury compounds shall be referred
41、 to thefacility hazardous waste coordinator.12. Keywords12.1 handling; mercury; mercury analysis; sampling; stor-ageBIBLIOGRAPHY(1) Bloom, N. S., Fresenius Journal of Analytical Chemistry, Vol 366,2000, pp. 438443.SUMMARY OF CHANGESSubcommittee D02.03 has identified the location of selected changes
42、to this standard since the last issue(D7482 15) that may impact the use of this standard. (Approved July 1, 2017.)(1) Information on the precision of two standard test methodsfor mercury determination has been added in a new Section 10.4Giles, H. N. and Mills, C. O., “Crude Oils: Their Sampling, Ana
43、lysis, andEvaluation,”ASTM International Press, West Conshohocken, PA, Manual 68, 2010.5Wilhelm, S. M., Kirchgessner, D. A., Liang, L., and Kariher, P. H., “Samplingand Analysis of Mercury in Crude Oil,” STP 1468, Elemental Analysis of Fuels andLubricants: Recent Advances and Future Prospects, Nadka
44、rni, R. A., Ed., ASTMInternational Press, West Conshohocken, PA, 2005.D7482 174ASTM International takes no position 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 vali
45、dity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This 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 comm
46、ents 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
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48、opies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 175
