ASTM D6520-2006 Standard Practice for the Solid Phase Micro Extraction (SPME) of Water and its Headspace for the Analysis of Volatile and Semi-Volatile Organic Compounds《挥发和半挥发性有机复.pdf
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1、Designation: D 6520 06Standard Practice forthe Solid Phase Micro Extraction (SPME) of Water and itsHeadspace for the Analysis of Volatile and Semi-VolatileOrganic Compounds1This standard is issued under the fixed designation D 6520; the number immediately following the designation indicates the year
2、 oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers procedures for the extraction ofvo
3、latile and semi-volatile organic compounds from water andits headspace using solid-phase microextraction (SPME).1.2 The compounds of interest must have a greater affinityfor the SPME-absorbent polymer or adsorbent or combinationsof these than the water or headspace phase in which theyreside.1.3 Not
4、all of the analytes that can be determined by SPMEare addressed in this practice. The applicability of the absor-bent polymer, adsorbent, or combination thereof, to extract thecompound(s) of interest must be demonstrated before use.1.4 This practice provides sample extracts suitable forquantitative
5、or qualitative analysis by gas chromatography(GC) or gas chromatography-mass spectrometry (GC-MS).1.5 Where used, it is the responsibility of the user to validatethe application of SPME to the analysis of interest.1.6 The values stated in SI units are to be regarded as thestandard.1.7 This standard
6、does not purport 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. For specific hazardstatements, s
7、ee Section 10.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD 3856 Guide for
8、 Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data3D 4448 Guide for Sampling Ground-Water MonitoringWells3. Terminology3.1 DefinitionsFor definitions of term
9、s used in this prac-tice, refer to Terminology D 1129.4. Summary of Practice4.1 This practice employs adsorbent/liquid or adsorbent/gasextraction to isolate compounds of interest.An aqueous sampleis added to a septum-sealed vial. The aqueous phase or itsheadspace is then exposed to an adsorbent coat
10、ed on a fusedsilica fiber. The fiber is desorbed in the heated injection port ofa GC or GC-MS or the injector of an HPLC.4.2 The desorbed organic analytes may be analyzed usinginstrumental methods for specific volatile or semi-volatileorganic compounds. This practice does not include sampleextract c
11、lean-up procedures.5. Significance and Use5.1 This practice provides a general procedure for thesolid-phase microextraction of volatile and semi-volatile or-ganic compounds from an aqueous matrix or its headspace.Solid sorbent extraction is used as the initial step in theextraction of organic consti
12、tuents for the purpose of quantify-ing or screening for extractable organic compounds.5.2 Typical detection limits that can be achieved usingSPME techniques with gas chromatography with flame ioniza-tion detector (FID), electron capture detector (ECD), or with amass spectrometer (MS) range from mg/L
13、 to g/L. Thedetection limit, linear concentration range, and sensitivity ofthe test method for a specific organic compound will dependupon the aqueous matrix, the fiber phase, the sample tempera-ture, sample volume, sample mixing, and the determinativetechnique employed.1This practice is under the j
14、urisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved July 1, 2006. Published July 2006. Originally approvedin 2000. Last previous edition approved in 2000 as D 6520 00.2For re
15、ferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO
16、Box C700, West Conshohocken, PA 19428-2959, United States.5.3 SPME has the advantages of speed, no desorptionsolvent, simple extraction device, and the use of small amountsof sample.5.3.1 Extraction devices vary from a manual SPME fiberholder to automated commercial device specifically designedfor S
17、PME.5.3.2 Listed below are examples of organic compounds thatcan be determined by this practice. This list includes both highand low boiling compounds. The numbers in parentheses referto references at the end of this standard.Volatile Organic Compounds (1,2,3)Pesticides, General (4,5)Organochlorine
18、Pesticides (6)Organophosphorous Pesticides (7,8)Polyaromatic Hydrocarbons (9,10)Polychlorinated biphenyls (10)Phenols (11)Nitrophenols (12)Amines (13)5.3.3 SPME may be used to screen water samples prior topurge and trap extraction to determine if dilution is necessary,thereby eliminating the possibi
19、lity of trap overload.6. Principles of SPME6.1 SPME is an equilibrium technique where analytes arenot completely extracted from the matrix. With liquid samples,the recovery is dependent on the partitioning or equilibrium ofanalytes among the three phases present in the sampling vial:the aqueous samp
20、le and headspace (Phase 1), the fiber coatingand aqueous sample (Phase 2), and the fiber coating and theheadspace (Phase 3):Phase 1! K15 CL/Cg(1)Phase 2! K25 CF/CL(2)Phase 3! K35 CF/CG(3)where CL,CGand CFare the concentrations of the analyte inthese phases.6.1.1 Distribution of the analyte among the
21、 three phases canbe calculated using the following:C0VL5 CGVG1 CLVL1 CFVF(4)6.1.2 Concentration of analyte in fiber can be calculatedusing the following:CF5 C0VLK1K2/VG1 K1VL1 K1K2VF(5)7. Interferences7.1 Reagents, glassware, septa, fiber coatings and othersample processing hardware may yield discre
22、te artifacts orelevated baselines that can cause poor precision and accuracy.7.1.1 Glassware should be washed with detergent, rinsedwith water, and finally rinsed with distilled-in-glass acetone.Air dry or in 103C oven. Additional cleaning steps may berequired when the analysis requires levels of g/
23、L or below.Once the glassware has been cleaned, it should be usedimmediately or stored wrapped in aluminum foil (shiny sideout) or under a stretched sheet of PTFE-fluorocarbon.7.1.2 Plastics other than PTFE-fluorocarbon should beavoided. They are a significant source of interference and canadsorb so
24、me organics.7.1.3 A field blank prepared from water and carried throughsampling, subsequent storage, and handling can serve as acheck on sources of interferences from the containers.7.2 When performing analyses for specific organic com-pounds, matrix interferences may be caused by materials andconst
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