ASTM D6438-2005(2010) 6875 Standard Test Method for Acetone Methyl Acetate and Parachlorobenzotrifluoride Content of Paints and Coatings by Solid Phase Microextraction-Gas Chromato.pdf
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1、Designation: D6438 05 (Reapproved 2010)Standard Test Method forAcetone, Methyl Acetate, and ParachlorobenzotrifluorideContent of Paints, and Coatings by Solid PhaseMicroextraction-Gas Chromatography1This standard is issued under the fixed designation D6438; the number immediately following the desig
2、nation indicates 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is for the det
3、ermination of acetone,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, an
4、d urethane solvent-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 i
5、t suitable for 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
6、are included in 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
7、 prior to use.2. Referenced Documents2.1 ASTM Standards:2D3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD6133 Test Method for Acetone, p-Chlorobenzotrifluoride,MethylAcetate or t-ButylAcetate Content of Solventborneand Waterborne Paints, Coatings, Resins, and Raw Mate-rials b
8、y Direct Injection Into a Gas ChromatographE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals33. Terminology3.1 Abbreviations:3.1.1 PCBTFparachlorobenzotrifluoride,(4-chlorobenzotrifluoride)3.1.2 MCBTFmetachlorobenzotrifluoride(
9、3-chlorobenzotrifluoride)3.1.3 SPMEsolid phase microextraction3.1.4 VOCvolatile organic compound3.1.5 PEG/DVBpolyethylene glycol/divinylbenzene3.1.6 FIDflame ionization detector3.1.7 MSmass selective or mass spectral3.1.8 SIMselected ion monitoring3.1.9 GCgas chromatograph3.1.10 Srrepeatability stan
10、dard deviations3.1.11 SRreproducibility standard deviations3.1.12 rrepeatability, 95 % confidence limit3.1.13 Rreproducibility, 95 % confidence limit4. Summary of Test Method4.1 A suitable aliquot of whole solvent-borne paint isinternally standardized and diluted with dioctyl phthalate. Theheadspace
11、 of this solution is sampled with an SPME fiber,which is then thermally desorbed 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 Us
12、e5.1 In order to calculate the volatile organic content (VOC)of paints containing 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. Each1T
13、his test method 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 Dec. 1, 2010. Published December 2010. Original
14、lyapproved in 1999. Last previous edition approved in 2005 as D6438 99 (2005).DOI: 10.1520/D6438-05R10.2For 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
15、 Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.analyte is measured with respect to a unique int
16、ernal standard.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 standard pairs behave very nearly as single solventswith respect to evaporation rate and adsorption ra
17、te 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 ability of an analyst to weigh a paint sample and internalstandard, corresponding to the analyte of i
18、nterest, 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 system isnever compromised.6. Apparatus6.1 Manual SPME Holder,4fitted with partially crosslinkedpol
19、yethylene 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. Temperature programming capability is desirable, butisothermal operations may be utilized.6.2.1 For F
20、ID instrument conditions, see Table 1.6.2.2 Inlet Liner, 0.75-mm should be placed in the injectionport.46.2.3 IntegratorAny electronic integrator that can accu-rately quantify a gas chromatographic peak area is acceptable.6.3 Gas Chromatograph, Mass Selective (MS) DetectionAny capillary gas chromato
21、graph 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 instrument conditions, see Table 2.6.3.2 Inlet liner, 0.75-mm, should be placed in the injectionport.4
22、6.3.3 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 conditionedaccording to the manufacturers recommendation. The col-umns may then be used indefinitely without furth
23、er 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 use.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all te
24、sts. 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 available.5Other grades may beused, provided it is first ascertained that the reagent is ofsuff
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