1、Designation: D 7049 04Standard Test Method forMetal Removal Fluid Aerosol in Workplace Atmospheres1This standard is issued under the fixed designation D 7049; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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 covers a procedure for the determina-tion of both total collected particulate matter and extractablemass metal r
3、emoval 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 metal removal f
4、luids.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. Refere
5、nced Documents2.1 ASTM Standards:2D 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 3195 Practice for Rotameter CalibrationD 3670 Guide for Determination of Precision and Bias ofMethods of Committee D-22D 4532 Test Method for Respirable Dust in WorkplaceAtmospheresD 5337 Practice f
6、or Flow Rate Calibration of PersonalSampling PumpsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Government Standards:29 CFR 1910.1000 Air Contaminants329 CFR 1910.1450 Occupational Exposure to HazardousChemicals in Laboratories32.3 NIOSH Documen
7、t:Method 0500 NIOSH Manual of Analytical Methods(NMAM), 4th Ed43. Terminology3.1 For definitions of terms relating to this test method, referto Terminology D 1356.3.2 Definitions of Terms Specific to This Standard:3.2.1 breathing zone, nthe workers breathing zone con-sists of a hemisphere 300-mm rad
8、ius 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, the 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.Thi
9、s 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-tion 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
10、field blanks being submitted for eachsampling day.3.2.4 metal removal fluids, nthe subset of metal workingfluids that are used for wet machining or grinding to producethe finished part. Metal removal fluids are often characterizedas straight, soluble, semisynthetic, and synthetic.3.2.4.1 DiscussionM
11、etal removal fluids addressed by thispractice include straight or neat oils, not intended for furtherdilution with water, and water-miscible soluble oils, semisyn-thetics, and synthetics, which are intended to be diluted withwater before use. Metal removal fluids become contaminatedduring use in the
12、 workplace with a variety of workplacesubstances including, but not limited to, abrasive particles,tramp oils, cleaners, dirt, metal fines and shavings, dissolvedmetal and hard water salts, bacteria, fungi, microbiologicaldecay products, and waste. These contaminants can causechanges in the lubricit
13、y and cooling ability of the metalremoval fluid as well as have the potential to adversely affect1This test method is under the jurisdiction of ASTM Committee D22 onSampling and Analysis and is the direct responsibility of Subcommittee D22.04 onWorkplace Atmospheres.Current edition approved May 1, 2
14、004. Published June 2004.2For 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.3Available from U.S. Government Prin
15、ting 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 Drive, PO Box C700, West Conshohocken, P
16、A 19428-2959, United States.the health and welfare of employees in contact with thecontaminated metal removal fluid.3.2.5 total particulate matter, nthe mass of materialsampled through the 4-mm inlet of a standard 37-mm filtercassette when operated at 2.0 L/min.3.2.5.1 DiscussionWhile this is the tr
17、aditional use of thisterm, it should be recognized that this is not a measure of theinhalable particulate mass.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
18、matter concen-tration is calculated from the 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
19、 the loss of mass following extractionand the 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. Significan
20、ce and Use5.1 This test method covers the gravimetric 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 t
21、est method provides an extension to current 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 abr
22、oad spectrum of solvent polarity to remove any 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 meth
23、od does not address the loss of semivola-tile 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 extrac
24、table mass concentration measurement im-proves 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 ar
25、e insolublein either extraction solvent mixture 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 sa
26、mpling.6.4.1 Samples of workplace atmospheres 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 ar
27、e lost from the filterduring the extraction 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 fil
28、tercassette for a full work shift (8 h).7.1.2 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 filtercas
29、sette to the worker for breathing zone sampling.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
30、 flowrates (for example, bubble flow meter, dry seal flow meter, orburette and stopwatch).7.1.7 Rotameter, calibrated in accordance with PracticeD 3195 for field check of sampler flow rate.7.1.8 Weighing Room, with temperature and humidity con-trol to allow weighing under reproducible environmentalc
31、onditions of 22 6 2C and 65 % relative humidity 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.7Harper, M., “A Simplified Procedure for the Extraction of Metalworking FluidSamples in Accordance with
32、Provisional ASTM/NIOSH Methods,” AIHAJ, 63,2002, pp. 488-492.D704904311.2 Maintenance and repairs of the sampling and analyticalequipment should be performed according to the recommen-dations of the manufacturer and should be documented inmaintenance records.11.3 The air flow rate calibration shall
33、be performed accord-ing to Practice D 5337.11.4 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 Procedure12.1 Allow the filters to warm to ambient laboratory tem-perature. Clean the ext
34、erior of the filter cassette (7.1.2) with amoist lintless towel to avoid sample contamination.12.2 Remove the tape from the cassette.12.3 Open the filter cassette (7.1.2) and carefully removethe filter (7.1.3) from the holder by inserting a rod through theoutlet and against the filter support.12.4 D
35、esiccate 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 (7.1.8) for a minimum of 2 h.12.6 Place the filter under a210Po antistatic strip (7.1.9.1). Asec
36、ond 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 was used for the initial weighing.12.8 Place the filter in the filter funnel (7.1.12).12.9 Apply
37、 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 Apply 10 mL of the 1:1 v/v blend of methanol:waterto the filter and extract in the same manner as
38、 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 least one minute contacttime.NOTE 1If desired, the solvent washings may be quantitatively col-lect
39、ed 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 aid in drying.12.13.1 If more rapid removal of solvent is desired, filterscan be placed on a sli
40、ghtly 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.12.15 Place the filter under a210Po antistatic strip (7.1.9.1).A second antistatic strip should b
41、e 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 weighings.12.17 Follow the same procedure (12.1-12.16) for the fieldblanks.12.18 Perform laborator
42、y 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 laboratoryand field blanks and instrument calibrations.13. Calculation13.1 Mass of total particul
43、ate 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 change,8andMTP= total particulate mass.13.2 Sample volume during collection:Vs5 Q 3 T/1000 (2)w
44、here: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 mass from Eq 1,VS= sample volume in m3from Eq 2, andCTP= total particulate matter concentration in
45、 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 extractable mass concentration:CE5 ME/VS(5)where:ME= extractable mass from Eq 4,VS= sample volume from Eq
46、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 quantitation for total particulate matter:LOQ 5 10 3 STDFB(7)8A pooled mean field blank mass chan
47、ge can be used for a set of filters (12.17).D7049044where: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 Limit of
48、 quantitation for extractable mass:LOQ 5 10 3 STDEB(9)where:STDEB= standard deviation of laboratory extractionblanks, andLOQ = limit of quantitation.14. Report14.1 Report total particulate concentration (13.3), extract-able mass concentration (13.5), limit of detection for totalparticulate matter (1
49、3.6), 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 Analytical 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 0500 by red
