ASTM D6438-2005 Standard Test Method for Acetone Methyl Acetate and Parachlorobenzotrifluoride Content of Paints and Coatings by Solid Phase Microextraction-Gas Chromatography《用固相微.pdf
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1、Designation: D 6438 05Standard Test Method forAcetone, Methyl Acetate, and ParachlorobenzotrifluorideContent of Paints, and Coatings by Solid PhaseMicroextraction-Gas Chromatography1This standard is issued under the fixed designation D 6438; the number immediately following the designation indicates
2、 the year 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 test method is for the determination of a
3、cetone,methyl acetate, or parachlorobenzotrifluoride (PCBTF), orcombination of any of the three, in paints and coatings, by solidphase microextraction (SPME) headspace sampling, and sub-sequent injection into a gas chromatograph. It has beenevaluated for cellulose nitrate, acrylic, and urethane solv
4、ent-borne systems. The established working range of this testmethod is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %;parachlorobenzotrifluoride, 10 to 17 %. There is no reason tobelieve that it will not work outside these ranges. A minormodification of this test method would make it suitable for
5、theanalysis of the same analytes in water-borne coatings (see Note1).NOTE 1Water-borne paints are internally standardized and dilutedwith water followed by addition of solid sodium chloride.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in
6、 thisstandard.1.3 This standard 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.2
7、. Referenced Documents2.1 ASTM Standards:2D 3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD 6133 Test Method for Acetone Content,p-Chlorobenzotrifluoride, Methyl Acetate or t-Butyl AcetateContent of Solventborne and Waterborne Paints, Coatings,Resins, and Raw Materials by Dir
8、ect Injection into A GasChromatographE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals3. Terminology3.1 Abbreviations:PCBTF parachlorobenzotrifluoride,(4-chlorobenzotrifluoride)MCBTF metachlorobenzotrifluoride(3-chlorobenzotri
9、fluoride)SPME solid phase microextractionVOC volatile organic compoundPEG/DVB polyethylene glycol/divinylbenzeneFID flame ionization detectorMS mass selective or mass spectralSIM selected ion monitoringGC gas chromatographSr repeatability standard deviationsSR reproducibility standard deviationsr re
10、peatability, 95 % confidence limitR reproducibility, 95 % confidence limit4. Summary of Test Method4.1 A suitable aliquot of whole solvent-borne paint isinternally standardized and diluted with dioctyl phthalate. Theheadspace of this solution is sampled with an SPME fiber,which is then thermally des
11、orbed in the injection port of a gaschromatograph onto a suitable capillary column. Either a flameionization or mass specific detector may be used to measurepeak areas of analytes and internal standards.5. Significance and Use5.1 In order to calculate the volatile organic content (VOC)of paints cont
12、aining EPA exempt solvents, it is necessary toknow the acetone, methyl acetate, or parachlorobenzotrifluo-ride content. This gas chromatographic test method provides asimple and direct way for measuring these solvents. Eachanalyte is measured with respect to a unique internal standard.1This test met
13、hod is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1, 2005. Published July 2005. Originally approvedin 19
14、99. Last previous edition approved in 1999 as D 6438 99.2For referenced 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.1Copy
15、right ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.For acetone, the internal standard used is acetone-d6, formethyl acetate it is methyl acetate-d3, and for PCBTF it ismetachlorobenzotrifluoride (MCBTF). These unique analyte/internal standar
16、d pairs behave very nearly as single solventswith respect to evaporation rate and adsorption rate onto acoated silica fiber (SPME) but are separable on a gas chro-matograph (GC) capillary column. The only critical analyticaltechnique required for successfully performing this test methodis the abilit
17、y of an analyst to weigh a paint sample and internalstandard, corresponding to the analyte of interest, into a septumcapped vial. After weighing, solvent evaporation has no effecton the final value of the determination. Since whole paint is notinjected into the gas chromatograph, the analytical syst
18、em isnever compromised.6. Apparatus6.1 Manual SPME Holder,3fitted with partially crosslinkedpolyethylene glycol/divinylbenzene (PEG/DVB) fiber assem-bly, 65m film thickness.6.2 Gas Chromatograph, FID DetectionAny capillary gaschromatograph equipped with a flame ionization detector maybe used. Temper
19、ature programming capability is desirable, butisothermal operations may be utilized.6.2.1 For FID instrument conditions, see Table 1.6.2.2 Inlet Liner, 0.75-mm should be placed in the injectionport.36.2.3 IntegratorAny electronic integrator that can accu-rately quantify a gas chromatographic peak ar
20、ea is acceptable.6.3 Gas Chromatograph, Mass Selective (MS) DetectionAny capillary gas chromatograph equipped with a mass selec-tive detector may be used. The detector must be capable ofmeasuring in the selected ion monitoring (SIM) mode at dwelltimes of 100 milliseconds or less.6.3.1 For MS instrum
21、ent conditions, see Table 2.6.3.2 Inlet liner, 0.75-mm, should be placed in the injectionport.36.3.3 The instrument should have a software data system toallow extraction and integration of the SIM ions.7. Column and Fiber Conditioning7.1 Either or both capillary columns should be conditionedaccordin
22、g to the manufacturers recommendation. The col-umns may then be used indefinitely without further condition-ing.7.2 The SPME fiber should be conditioned and used accord-ing to the manufacturers recommendation.7.3 The SPME fiber should be inserted into a 260 Cinjection port for 30 s prior to daily us
23、e.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are
24、available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.8.2 Carrier Gas, Helium of 99.995 % or higher purity.8.3 Acetone -d6, 99.9 % isotopic purity.8.4 Methyl Acetate -d3
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