1、Designation: D7049 04 (Reapproved 2010)Standard Test Method forMetal Removal Fluid Aerosol in Workplace Atmospheres1This standard is issued under the fixed designation D7049; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 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 covers a procedure for the determina-tion of both total collected particulate matter and extracta
3、blemass metal removal fluid aerosol concentrations in the range of0.05 to 5 mg/m3in workplace atmospheres.1.2 This test method describes a standardized means ofcollecting worker exposure information that can be comparedto existing exposure databases, using a test method that is alsomore specific to
4、metal removal fluids.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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 stand
5、ard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1356 Terminology Relating to Sampling and Analysis ofAtmospheresD3195 Practice for Rotameter CalibrationD3670 Guide for Determ
6、ination of Precision and Bias ofMethods of Committee D22D4532 Test Method for Respirable Dust in WorkplaceAtmospheres Using Cyclone SamplersD5337 Practice for Flow Rate Calibration of PersonalSampling PumpsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Meth
7、od2.2 Government Standards:29 CFR 1910.1000 Air Contaminants329 CFR 1910.1450 Occupational Exposure to HazardousChemicals in Laboratories32.3 NIOSH Document:Method 0500 NIOSH Manual of Analytical Methods(NMAM), 4th Ed43. Terminology3.1 For definitions of terms relating to this test method, referto T
8、erminology D1356.3.2 Definitions of Terms Specific to This Standard:3.2.1 breathing zone, nthe workers breathing zone con-sists of a hemisphere 300-mm radius extending in front of theface, centered on the midpoint of a line joining the ears; thebase of the hemisphere is a plane through this line, th
9、e top ofthe head and the larynx.3.2.2 extractable mass, nthe material removed by liquidextraction of the filter using a mixed-polarity solvent mixture.This mass is an approximation of the metal removal fluidportion of the workplace aerosol.3.2.3 filter set, na group of filters from the same produc-t
10、ion lot that are weighed and assembled into the filter cassettesat one time. The filter set may be used for sampling on multipledays with the appropriate field blanks being submitted for eachsampling day.3.2.4 metal removal fluids, nthe subset of metal workingfluids that are used for wet machining o
11、r grinding to producethe finished part. Metal removal fluids are often characterizedas straight, soluble, semisynthetic, and synthetic.3.2.5 DiscussionMetal removal fluids addressed by thispractice include straight or neat oils, not intended for furtherdilution with water, and water-miscible soluble
12、 oils, semisyn-thetics, and synthetics, which are intended to be diluted withwater before use. Metal removal fluids become contaminatedduring use in the workplace with a variety of workplacesubstances including, but not limited to, abrasive particles,tramp oils, cleaners, dirt, metal fines and shavi
13、ngs, dissolvedmetal and hard water salts, bacteria, fungi, microbiologicaldecay products, and waste. These contaminants can causechanges in the lubricity and cooling ability of the metalremoval fluid as well as have the potential to adversely affectthe health and welfare of employees in contact with
14、 thecontaminated metal removal fluid.1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved April 1, 2010. Published June 2010. Originallyapproved in 2004. Last previous
15、edition approved in 2004 as D7049 - 04. DOI:10.1520/D7049-04R10.2For 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 websi
16、te.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.4Available from National Institute for Occupational Safety and Health, 4676Columbia Pkwy., Cincinnati, OH 45226.1Copyright ASTM International, 100 Barr Harbor D
17、rive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Test Method4.1 Workplace air is drawn into a 37-mm filter cassettecontaining a tared polytetrafluoroethylene (PTFE) filter for ameasured period of time. The total particulate matter concen-tration is calculated from the
18、 mass gain of the filter and thevolume of air sampled.4.2 The filter is extracted with a ternary mixture of bothnonpolar and polar solvents, a second mixture of methanol andwater, dried, and reweighed. The extractable mass concentra-tion is calculated from the loss of mass following extractionand th
19、e volume of air sampled.4.3 As a cost-control procedure, the nonspecific total par-ticulate matter concentration may be used in place of theextractable mass if the total particulate concentration is accept-able to the user of this test method.5. Significance and Use5.1 This test method covers the gr
20、avimetric determinationof metal removal fluid aerosol concentrations in workplaceatmospheres.5.2 The test method provides total particulate matter con-centrations for comparison with historical exposure databasescollected with the same technology.5.3 The test method provides an extension to current
21、non-standardized methods by adding an extractable mass concen-tration which reduces interferences from nonmetal removalfluid aerosols.5.4 The test method does not address differences betweenmetal removal fluid types, but it does include extraction with abroad spectrum of solvent polarity to remove a
22、ny of the currentfluid formulations from insoluble background aerosol ad-equately.55.5 The test method does not identify or quantify anyspecific putative toxins in the workplace that can be related tometal removal fluid aerosols or vapors.5.6 The test method does not address the loss of semivola-til
23、e compounds from the filter during or after collection.6. Interferences6.1 The total particulate matter portion of the test method isnot specific to metal removal fluid in the workplace and issubject to positive bias by other aerosol sources.6.2 The extractable mass concentration measurement im-prov
24、es the specificity of the test method by eliminatinginsoluble background aerosol from the determination of themetal removal fluid aerosol concentration. This is an importantconsideration at low-exposure limits.6.3 Any metal removal fluid components that are insolublein either extraction solvent mixt
25、ure will not be measured in theextractable mass fraction.6.4 The total particulate and extractable mass concentra-tions measured with this test method are subject to a negativebias to the extent that semivolatile compounds are lost from thefilter during sampling.6.4.1 Samples of workplace atmosphere
26、s in which metalremoval fluids containing lower viscosity petroleum fractionsor volatile alkanolamines are used may be particularly subjectto this negative bias both during sampling and during storagetime before analysis.6.5 Any insoluble materials that are lost from the filterduring the extraction
27、process will be reported as extractablemass resulting in a positive bias.7. Apparatus7.1 The sampling unit consists of a pump and filter cassette.7.1.1 Pump, a constant-flow personal sampling pump ca-pable of a flow rate of 2.0 L/min (65 %) through the filtercassette for a full work shift (8 h).7.1.
28、2 Filter Cassette, a closed-face (4-mm opening) two- orthree-piece 37-mm filter cassette with filter-support pad andinlet and outlet plugs.7.1.3 Filter, the filter shall be a 2-m PTFE membrane filter.7.1.4 Suitable means of attaching the pump and filtercassette to the worker for breathing zone sampl
29、ing.7.1.5 Field Blank, a filter cassette prepared for sampling thathas been taken to the workplace and handled in the samemanner as the analytical filters, but which has not had any airdrawn through it.7.1.6 Precision Flow Meter, for calibration of sampler flowrates (for example, bubble flow meter,
30、dry seal flow meter, orburette and stopwatch).7.1.7 Rotameter, calibrated in accordance with PracticeD3195 for field check of sampler flow rate.7.1.8 Weighing Room, with temperature and humidity con-trol to allow weighing under reproducible environmentalconditions of 22 6 2C and 65 % relative humidi
31、ty in a rangeof 30 to 55 %.7.1.9 Analytical Balance, capable of weighing to 60.001mg.7.1.9.1 Antistatic Strips,of210Po + 5 %) during the sample period.11.2 Maintenance and repairs of the sampling and analyticalequipment should be performed according to the recommen-dations of the manufacturer and sh
32、ould be documented inmaintenance records.11.3 The air flow rate calibration shall be performed accord-ing to Practice D5337.11.4 Check the calibration of the analytical balance (7.1.9)daily using National Institute of Standards and TechnologyClass S-1.1 or ASTM Class 1 masses.12. Analytical Procedur
33、e12.1 Allow the filters to warm to ambient laboratory tem-perature. Clean the exterior of the filter cassette (7.1.2) with amoist lintless towel to avoid sample contamination.D7049 04 (2010)312.2 Remove the tape from the cassette.12.3 Open the filter cassette (7.1.2) and carefully removethe filter (
34、7.1.3) from the holder by inserting a rod through theoutlet and against the filter support.12.4 Desiccate the filter (7.1.3) in a chemical desiccator(7.1.11) over CaSO4for no more than 2 h. Do not desiccate ina vacuum desiccator.12.5 Equilibrate or condition the filters (7.1.3) in the weigh-ing room
35、 (7.1.8) for a minimum of 2 h.12.6 Place the filter under a210Po antistatic strip (7.1.9.1).Asecond antistatic strip should be placed in the balance weighingchamber, if possible.12.7 Weigh the filter (7.1.3) and record the mass to thenearest 0.001 mg (m2) using the same analytical balance (7.1.9)as
36、was used for the initial weighing.12.8 Place the filter in the filter funnel (7.1.12).12.9 Apply 10 mL of the ternary extraction solvent (8.5).Allow at least five minutes contact time.12.10 Apply vacuum to the filter funnel. Assure that solventvaporized does not contaminate the vacuum system.12.11 A
37、pply 10 mL of the 1:1 v/v blend of methanol:waterto the filter and extract in the same manner as in 12.10,allowing at least one minute contact time.12.12 Apply an additional 10 mL of the ternary solventmixture (8.5) to the filter and extract in the same manner asSteps 12.10 and 12.11, allowing at le
38、ast one minute contacttime.NOTE 1If desired, the solvent washings may be quantitatively col-lected for chemical analysis of specific contaminants.12.13 Rinse the inside of the extraction filter with a streamof the ternary solvent mixture (8.5) to return any insolubleparticulate to the filter and to
39、aid in drying.12.13.1 If more rapid removal of solvent is desired, filterscan be placed on a slightly warm, clean hot plate covered withnew aluminum foil or in a clean, dust-free vacuum oven not toexceed 50C for a few minutes.12.14 Equilibrate the filter (7.1.3) in the weighing room for2 h minimum.1
40、2.15 Place the filter under a210Po antistatic strip (7.1.9.1).A second antistatic strip should be placed in the balanceweighing chamber, if possible.12.16 Weigh the filter (7.1.3) and record the mass to thenearest 0.001 mg (m3) using the same analytical balance (7.1.9)as was used for the previous we
41、ighings.12.17 Follow the same procedure (12.1-12.16) for the fieldblanks.12.18 Perform laboratory blank (7.1.13) analyses for totalparticulate matter and extractable mass at least on each new lotof filters or solvents using the procedure in 12.1-12.16.12.19 Maintain appropriate QA/QC charts on all l
42、aboratoryand field blanks and instrument calibrations.13. Calculation13.1 Mass of total particulate aerosol collected on thesample filter (all masses expressed in mg):MTP5 m22 m1! 2 mB(1)where:m1= tare mass of the filter before sampling,m2= mass of the filter after sampling,mB= mean field blank mass
43、 change,8andMTP= total particulate mass.13.2 Sample volume during collection:Vs5 Q 3 T/1000 (2)where:Q = mean flow rate, L/min,T = sample time, min,1000 = conversion of L to m3, andVS= sample volume in m3of air.13.3 Total particulate matter concentration:CTP5 MTP/VS(3)where:MTP= total particulate ma
44、ss from Eq 1,VS= sample volume in m3from Eq 2, andCTP= total particulate matter concentration in mg/m3.13.4 Extractable mass:ME5 m22 m3! 2 mE(4)where:m2= mass of the filter after sampling,m3= mass following solvent extraction,mE= mean lab extraction blank, andME= extractable mass.13.5 The extractabl
45、e mass concentration:CE5 ME/VS(5)where:ME= extractable mass from Eq 4,VS= sample volume from Eq 2, andCE= extractable mass concentration.13.6 Limit of detection for total particulate matter:LOD 5 3 3 STDFB(6)where:STDFB= standard deviation of field blanks, andLOD = limit of detection.13.7 Limit of q
46、uantitation for total particulate matter:LOQ 5 10 3 STDFB(7)where:STDFB= standard deviation of field blanks, andLOQ = limit of quantitation.13.8 Limit of detection for extractable mass:LOD 5 3 3 STDEB(8)where:STDEB= standard deviation of laboratory extractionblanks, andLOD = limit of detection.13.9
47、Limit of quantitation for extractable mass:LOQ 5 10 3 STDEB(9)8A pooled mean field blank mass change can be used for a set of filters (12.17).D7049 04 (2010)4where:STDEB= standard deviation of laboratory extractionblanks, andLOQ = limit of quantitation.14. Report14.1 Report total particulate concent
48、ration (13.3), extract-able mass concentration (13.5), limit of detection for totalparticulate matter (13.6), limit of quantitation for total particu-late matter (13.7), limit of detection for extractable mass (13.8)and limit of quantitation for extractable mass (13.9).15. Precision and Bias915.1 An
49、alytical Range, 0.05 to 5 mg per sample (approxi-mately 0.2 to 5 mg/m3for full-shift sample).15.2 Estimated Limit of Detection:1015.2.1 Total Particulate MatterSee Eq 6. While the fullvalidation of this test method is pending, NIOSH Method 0500reports a LOD of 30 g or a corresponding full-shift sampleLOD of 0.03 mg/m3. The test method described here improveson NIOSH Method 0500 by reducing the blank variabilitythrough the use of PTFE filter medium.1115.2.2 Extractable MassSee Eq 8. The LOD range forthis test method will be established during the validationprocess.15.3
