1、Designation: D 6333 98 (Reapproved 2004)e1Standard Practice forCollection of Dislodgeable Pesticide Residues from Floors1This standard is issued under the fixed designation D 6333; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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.e1NOTEEditorial changes were made in paragraphs 3.1.1, 7.5.2, and Footnote 4 in April 2004.1. Scope1.1 This practice co
3、vers a procedure for collection ofdislodgeable pesticide residues from indoor floor surfaces.1.2 This practice and the sampling methodology describedare applicable to bare floors or covered floor surfaces, forexample, carpeting and vinyl flooring.1.3 This practice and the sampling methodology descri
4、bedare applicable to all pesticides listed in Practice D 4861whether applied directly to the floor surface or transportedthere by migration within the room or tracked in fromoutdoors.1.4 Floor surfaces for which this practice has been success-fully applied include nylon plush carpeting, polypropylen
5、elevel-loop carpeting, and vinyl flooring.1.5 Sample analysis will be dependent upon the nature ofthe pesticides targeted and is beyond the scope of this practice;however, the analytical procedures discussed in PracticeD 4861 are applicable to this practice.1.6 The values stated in SI units are to b
6、e regarded as thestandard.1.7 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 pr
7、ior to its use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 4861 Practice for Sampling and Selection of AnalyticalTechniques for Pesticides and Polychlorinated Biphenylsin AirE 1 Specification for
8、 ASTM ThermometersE 337 Test Method for Measuring Humidity with a Psy-chrometer (the Measurement of Wet-Bulb and Dry-BulbTemperatures)3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, refer to Terminology D 1356.3.1.1 dislodgeable residuethat part of the residue of achemi
9、cal deposited on a solid surface that may be transferredby direct contact to human skin or clothing (sometimes calledtransferable residue).3.1.2 sampling traversethe distance from the startingpoint to the end point over which the sampling media contactsthe floor surface for collection of a single sa
10、mple.3.1.3 transfer coeffcientthe ratio of the amount of pesti-cide residue collected by the sampling media to the area of thesurface contacted by the media during a single samplingtraverse.3.1.4 transfer effciencythe ratio of the transfer coefficientto the pesticide surface loading determined by an
11、alysis ofdeposition coupons placed strategically on the test surfacebefore the pesticide application.4. Summary of Practice4.1 The sampling method described in this practice is takenfrom published work (1,2,3,4)3.4.2 Dislodgeable pesticide residues from floor surfaces arecollected by transfer to an
12、annular ring of polyurethane foam(PUF), which is rolled across the floor at a constant speed andapplied pressure.4.3 The PUF sampling ring is slipped over a cylindricalmetal axle that functions as the front wheel of the PUF rollerapparatus. The apparatus is typically constructed of aluminumand consi
13、sts of a frame with two permanent rear wheels and thedetachable axle cylinder on the front.4.4 Weights are attached to the roller frame to apply thedesired downward force on the PUF roller ring (samplingpressure). A total weight of 3.88 kg provides a sampling1This practice is under the jurisdiction
14、of ASTM Committee D22 on Samplingand Analysis of Atmospheres and is the direct responsibility of SubcommitteeD22.05 on Indoor Air.Current edition approved April 1, 2004. Published June 2004. Originallyapproved in 1998. Last previous edition approved in 1998 as D 6333 - 98.2For referenced ASTM standa
15、rds, 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.3The boldface numbers in parentheses refer to the list of references at the end ofthis s
16、tandard.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.pressure of 8300 Pa, corresponding approximately to that of a9 kg child crawling or walking.4.5 A handle is connected at the rear of the roller frame topush or pull the device a
17、cross the floor surface.4.6 A template or similar measuring device is used toidentify the area to be sampled. The axle cylinder is fitted witha clean PUF ring, and the roller is then pushed at a constant rateof approximately 10 cm/s over a distance of 1.0 m and thenimmediately pulled in the reverse
18、direction back over the samesampling area at the same rate of speed, ending at the originalstarting position.4.7 The PUF ring is removed from the detached axlecylinder and placed in a sealed container for transport to thelaboratory for analysis.4.8 The PUF ring is extracted and analyzed using specif
19、icanalytical procedures for the pesticides of interest. Typicalmethods involve Soxhlet extraction with analysis of extracts bygas chromatography/mass spectrometry (GC/MS), gaschromatography/electron capture detection (GC/ECD), orother techniques noted in Practice D 4861.5. Significance and Use5.1 Th
20、is practice may be used to estimate the potential forhuman exposure to pesticide residues that may be dislodgedfrom residential floor surfaces by dermal contact. The samplingdevice employed is designed to approximately replicate thepressure applied bya9kgchild crawling or walking on thefloor.5.2 Lab
21、oratory tests and field studies have shown that thetransfer coefficient of the sampling device for collection ofdried pesticide residues from nylon plush carpets is two tothree times higher than that of a dry hand (palm only) pressedten times at 7300 Pa over the same area of carpet (2,4,5).5.3 This
22、practice has been found suitable for use on plushand level loop carpets and vinyl flooring (2, 3).5.4 This practice does not describe procedures for evalua-tion of the safety of floor surfaces or the potential for humanexposure to dislodgeable pesticide residues. It is the usersresponsibility to eva
23、luate the data collected by this practice andmake such determinations in the light of other availableinformation.6. Interferences6.1 There are no known interferences to the collection ofdislodgeable pesticide residues from floors using this practice.The presence of excessive moisture levels in carpe
24、ting, as maybe the case shortly after a wet cleaning operation, may affectthe dislodgeability of residues, possibly yielding higher thannormal results.6.2 Analytical interferences may be caused by contaminantsin the sampling medium, solvents, and reagents and onglassware and other sampling or sample
25、 processing hardwarethat result in discrete artifacts and elevated baselines, or both,in the detector profiles. For potential analytical interferences,refer to Practice D 4861.7. Apparatus7.1 PUF Roller Sampler, (as shown in Fig. 1) may beconstructed by a machinist using primarily aluminum materi-al
26、s. The typical apparatus consists of a frame (12.4 by 25.4 cm)that is attached to a rear axle that holds a swivel joint in thecenter for attaching the handle and has two aluminum wheels(2.5-cm wide by 10.2-cm diameter). The distance between theoutside of the two wheels is 21.6 cm and between the ins
27、ide ofthe wheels is 16.5 cm. An aluminum cylinder (7.6-cm long by4.3-cm diameter) is attached to the front of the sampler frameby 6-mm diameter hex head axle bolts on the cylinder that fitinto slots on the frame. This cylinder serves as the front axleand also holds the PUF sampling medium (see 7.2).
28、 The frontaxle cylinder is secured in the slots by spring steel retainingFIG. 1 PUF Roller: A. In Position for Sampling. B. Axle Cylinder/Frame Assembly.D 6333 98 (2004)e12clips that permit easy attachment and removal of the cylinder.The handle for the sampler is two pieces that screw together(102-c
29、m long by 1.3-cm diameter, overall) and then screw intothe swivel joint on the rear axle. Two stainless steel blocks,each measuring 12.7 by 7.3 by 2.5 cm and having a combinedweight of 3.88 kg, are attached to the center of the framethrough holes that fit over 3-mm diameter threaded posts oneither s
30、ide of the frame. The weights are secured to the framewith hand-tightened knurled nuts.NOTE 1Although the use of stainless steel to construct the weights isnot required (other materials of similar density will suffice), the ease ofcleaning and resistance to corrosion make this metal very useful.7.2
31、PUF Sampling MediumThe sampling medium con-sists of an annular plug cut from a sheet of medium density(0.029 g/cm3) open-cell, polyether-type polyurethane foam,7.6-cm thick.NOTE 2This foam is the type used commercially in upholstery and iswidely used for air sampling. It is the same type as that des
32、cribed inPractice D 4861, but has a higher density.7.2.1 Cut the foam sheet stock with a high-speed cutting dielubricated with distilled water to produce an annular ring8.9-cm O.D. by 4.2-cm I.D. Alternatively, the PUF sheet stockmay be immersed in distilled water and compressed to achievesaturation
33、 prior to cutting.7.2.2 After cutting, immerse the rings in pesticide gradeacetone and compress to remove most of the distilled water.Repeat the process.7.2.3 Extract the rings with acetone in a Soxhlet extractorfor 24 h at 4 to 6 cycles/h, followed by a second extraction with5 % diethyl ether in n-
34、hexane for an additional 14 to 24 h at 4to 6 cycles/h. A final 24-h extraction with acetone is recom-mended to ensure that the PUF ring retains its shape.7.2.4 Upon completion of the Soxhlet extractions, transferthe PUF rings with solvent-rinsed tweezers into an open,pre-cleaned container (Refer to
35、Practice D 4861 for cleaning).7.2.5 Place containers with PUF rings inside a vacuumdrying oven and dry for 16 h under purified zero gradenitrogen.7.2.6 Place the dried rings in clean, sealed containers forstorage, preferably in an area protected from prolonged expo-sure to light.7.3 Guide BarA flat
36、bar or ruler approximately 1.4-mlong can be used to guide the sampler during a traverse over thefloor surface. For example, an aluminum bar 2.5-cm wide and6-mm thick may be used in this application. The bar is clearlymarked at the starting point and at 10-cm intervals along itslength up to and inclu
37、ding the ending point at the 1.0-m mark.The starting point is marked on the bar about 34 cm from oneend so that the wheels of the sampler will contact the bar whenthe front of the sampler is in place to begin a sampling traverse.7.3.1 Alternatively, a template may be constructed to serveas a guide f
38、or sampling. An example of such a template that hasbeen found useful may be constructed from two 168-cm longright-angled side bars made from extruded aluminum or othersuitable material with each side of the L-shaped bar having awidth of about 2.5 cm. The two angled sidebars are connectedat each end
39、with a 2.5-cm wide flat bar that is 21.5-cm long,thereby resulting in two tracks that will accommodate the rearwheels of the PUF roller with only a slight tolerance. Thethickness of the side and end bars is approximately 0.3 cm. Thevertical height of the side bars should be sufficient to keep thewhe
40、els on the track, for example 2.5 cm. The carpet surface isexposed through a central opening 163 by 16.5 cm in dimen-sion. The template is clearly marked at the starting point and at10-cm intervals along its length up to and including the endingpoint at the 1.0-m mark. The starting point is marked o
41、n thetemplate about 34 cm from one end so that the wheels of thesampler will remain upon the tracks with some room to sparewhen the front of the sampler is in position to begin a sampletraverse.7.4 Starting PlatformA thin (1.6-mm) aluminum sheet(33 by 25.4 cm) to be used as a platform to prevent con
42、tact ofthe PUF ring with the surface to be sampled before starting asampling traverse.7.5 Other Equipment:7.5.1 Tongs, large (23-cm long), scissor type, stainless steeltongs, or similar implements, for installing and removing thePUF rings from the sampler apparatus.7.5.2 GlovesProtective gloves, pow
43、der-free nitrile, latex,or polyvinyl acetate, are required to guard against potentiallyhazardous exposures and to minimize risk of cross contamina-tion between sampler apparatus and sampling media.7.5.3 Squeeze BottleA plastic (polytetrafluroethylene)squeeze bottle, 250500-mL volume, is filled with
44、solvent andis used to rinse the sampler apparatus that contacts thesampling media and the tongs used to install and remove themedia.7.5.4 Stopwatch.7.5.5 Clean Glass Jars, for the collection and storage ofsamples.7.5.6 Thermometer (see Specification E 1).7.5.7 Relative Humidity Meter (see Test Metho
45、d E 337).8. Reagents8.1 Acetone, pesticide quality.8.2 n-Hexane, pesticide quality.8.3 Diethyl Ether, analytical reagent grade, preserved with2 % ethanol.8.4 2-Propanol, pesticide quality.8.5 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is inten
46、ded thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.48.6 Purity of WaterReferences to distilled water shall beunderstood to mean distilled water, which is Type II reagentwater confo
47、rming to Specification D 1193.9. Sampling Procedure9.1 Sampling Layout:4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChe
48、micals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,MD.D 6333 98 (2004)e139.1.1 At least three samples should be collected in the roomto be monitored. Unless the monitoring protocol requiresotherwise, t
49、he areas to be sampled should be selected in amanner that reflects the average surface of the floor; typically,one sample should be taken near a doorway, one in the centerof the room, and one near a corner.NOTE 3The area chosen for sampling should be at least 30 cm fromwalls that may have received crack and crevice treatments.9.1.2 Identify the sampling area and mark the beginning andend of the 1.0-m sampling traverse with tape, chalk mark,guidebar, or another suitable visual indicator. For adequatecharacterization of a room, at minimum, three samples shouldbe tak
