1、Designation: E1645 01 (Reapproved 2016)1E1645 16Standard Practice forPreparation of Dried Paint Samples by Hotplate orMicrowave Digestion for Subsequent Lead Analysis1This standard is issued under the fixed designation E1645; the number immediately following the designation indicates the year oforig
2、inal 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 NOTECaution statements in 6.1.2, 6.1.2.1, 6.1.2.2, 6.2.4.4, 7.2.1, and 7.
3、2.2 were changed to Warning statementseditorially in January 2016.1. Scope1.1 This practice covers the sample preparation procedures for paint samples that are collected during the assessment,management or control of lead hazards.1.2 This practice describes the digestion procedures using a hot plate
4、 or microwave oven or apparatus for paint samples thatare to be analyzed for lead content.1.3 This practice covers the general considerations for quantitative sample extraction for total recoverable lead in dried paintsamples (either bulk paint or paint powder) using hot plate or microwave heating t
5、echniques, or both.1.4 This practice contains notes that are explanatory and not part of the mandatory requirements of the standard.1.5 This practice is based on two NIOSH Methods, 7082 and 7105, and on an EPA standard operating procedure for lead inpaint.1.6 The values stated in SI units are to be
6、regarded as standard. No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and d
7、etermine the applicability of regulatorylimitations prior to use. For specific precautionarywarning statements, see 6.1.2, 6.1.2.1, 6.1.2.2, 6.2.4.46.3.2.4, 7.2.1, and 7.2.2.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterE288 Specif
8、ication for Laboratory Glass Volumetric FlasksE969 Specification for Glass Volumetric (Transfer) PipetsE1605 Terminology Relating to Lead in BuildingsE1729 Practice for Field Collection of Dried Paint Samples for Subsequent Lead Determination2.2 ISO Documents:3ISO Guide 30 Reference materials - Sele
9、cted terms and definitionsISO 1042 Laboratory glassware - One-mark volumetric flasksISO 8655 Piston-operated volumetric apparatus - Part 1: Terminology, general requirements and user recommendations2.3 Other Documents:Environmental Protection Agency, NTIS Standard Operating Procedures for Lead in Pa
10、int by Hotplate- or Microwave-basedAcid Digestions andAtomicAbsorption or Inductively Coupled Plasma Emission Spectrometry ; U.S. EPA, ResearchTrianglePark, NC (1991). (NTIS No. PB92114172)PB92114172 Standard Operating Procedures for Lead in Paint by Hotplate- or1 This practice is under the jurisdic
11、tion of ASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead HazardsAssociated with Buildings.Current edition approved Jan. 1, 2016March 1, 2016. Published January 2016April 2016. Originally approved in 1994. Last previous edition approved in
12、 20072016 asE1465 01E1645 01 (2016)1(2007). DOI: 10.1520/E1645-01R16E01.10.1520/E1645-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summa
13、ry page on the ASTM website.3 Available from International Organization for Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,Switzerland, http:/www.iso.org.This document is not an ASTM standard and is intended only to provide the user of a
14、n ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as publi
15、shed by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Microwave-based Acid Digestions and Atomic Absorption or Inductively Coupled Plasma Emission Spectrometry4NIOSH Manual of Analytica
16、l Methods,NMAM 7082 and 7105 P.M. Eller and M.E. Cassinelli, Eds., 4th ed., Methods 7082and 7105; National Institute for Occupational Safety eachcertified value is accomplished by an uncertainty at a stated level of confidence. ISO Guide 303.1.9 sample seta group of samples (one or more).3.1.10 spik
17、ed sample or spiked duplicate samplea blank medium that contains no purposely added analyte to which a knownamount of analyte is added before preparation.3.1.10.1 DiscussionAnalysis results for these samples are used to provide information on the precision and accuracy of the overall process.4. Summ
18、ary of Practice4.1 Lead in dried paint samples (chips, powder, etc.) and so forth) is solubilized (extracted) by digestion with nitric acid andhydrogen peroxide facilitated by heat, or by a mixture of nitric acid and hydrochloric acid facilitated by microwave energy. (It isassumed that the paint sam
19、ples were collected in accordance with Practice E1729; however, this practice can be used for anycollected paint sample.) The lead content of the digested sample is then in a form ready for measurement.4 U.S. EPA, Research Triangle Park, NC (1991). Available from National Technical Information Servi
20、ce (NTIS), 5301 Shawnee Rd., Alexandria, VA 22312,http:/www.ntis.gov.5 P.M. Eller, and M.E. Cassinelli, Eds., National Institute for Occupational Safety 45226, Mail Stop C14, http:/www.cdc.gov/niosh.E1645 1625. Significance and Use5.1 Paint in buildings and related structures needs to be monitored f
21、or lead content in order to determine the potential leadhazard. Hence, effective and efficient methods are required for the preparation of paint samples that may contain lead.5.2 This practice may be used for the digestion of paint samples that are collected during various lead-hazard control and ri
22、skassessment activities associated with lead abatement in and around buildings and related structures. This practice is also suitablefor the digestion of paint samples collected from locations such as commercial buildings.5.3 This practice may be used to prepare samples that have been obtained in or
23、der to ensure compliance with laws that governlead content in paints.5.4 This practice may be used to prepare samples that have been collected for risk assessment purposes.5.5 This practice is intended for use with paint samples that are prepared for subsequent analysis by laboratory-basedquantitati
24、ve analytical methods.6. Apparatus6.1 Heating Equipment:6.1.1 Electric Hot Platesuitable for operation at surface temperatures up to at least 140C. A temperature of at least 100C,as measured by a thermometer placed inside a borosilicate glass container (on the hot plate) filled with digestion soluti
25、on, shouldbe attainable. (See Note 1.)NOTE 1Provided that the hot plate is capable of handling the extra heating required, use of a 12 to 25-mm (approximately 0.5 to 1-in.) thick aluminumplate placed on the burner head can help reduce the presence of hot spots common to electric hot plates.6.1.2 Mic
26、rowave Extraction Apparatus:WarningEnsure that manufacturers safety recommendations are followed.NOTE 2The procedure described is for microwave digestion systems with a temperature control system. Microwave digestion systems that areequipped only with a pressure control system or lower pressure vess
27、els, or both, may be used, provided that a prior assessment of the dissolution efficiencyis carried out.6.1.2.1 Microwave Digestion Systemdesigned for closed vessel digestion, with power output regulation, fitted with atemperature control system capable of sensing the temperature to within 62C, and
28、automatically adjusting the microwave poweroutput within 2 s. The microwave cavity shall be resistant to chemical attack, and equipped with exhaust ventilation for acid vaporprotection of the unit and operator. All electronics shall be protected against corrosion to ensure safe operation. Safety int
29、erlocks,to shut off magnetron power output, shall be contained within the oven door opening mechanism.WarningDomestic (kitchen) microwave ovens shall not be used, since there are very significant hazards associated with theiruse for the procedure described in this standard. For example, acid vapors
30、released into the cavity can corrode safety devices thatprevent the magnetron from shutting off when the door is opened, potentially exposing the operator to microwave energy. Also,the fumes generated can be extremely hazardous.NOTE 3A pressure control system is also very useful, since it provides a
31、 safeguard against the possibility of sample loss due to excessive pressurebuildup and partial venting of the sample vessels.6.1.2.2 Lined Sample Vesselsclosed, designed for carrying out microwave digestions, capable of withstanding a temperatureof at least 180C and with an internal volume of at lea
32、st 50 mL. 50 mL. The vessels must be transparent to microwave energy,and vessel liners shall be chemically inert. The vessels must be capable of withstanding high internal pressures (up to at least 3000kPa) and temperatures (up to at least 180C).Vessels shall also be equipped with a safety relief va
33、lve or disc that will prevent vesselrupture or ejection of the vessel cap. Such vessels consist of an inner liner and cover made of a microwave transparent andchemically resistant material (usually a fluorocarbon polymer such as tetra-fluoromethoxil polymer (TFM), which contains andisolates the samp
34、le solution from a high strength, outer pressure structure. Other types of sample vessels designed to operate atequivalent or higher temperatures or pressures, or both, may be used.WarningFor closed vessel designs, the material from which the outer vessels are made is usually not as chemically inert
35、 asthe liner material. Since the outer vessels provide the strength required to withstand the high pressures within the inner liners, theymust be inspected regularly to check for any chemical or physical degradation.6.2 Glassware and Supplies:6.2.1 Apparatus-Hot Plate Digestion:6.2.1.1 Borosilicate
36、glass beakers, 125-mL or 50-mL with watchglass covers,6.2.1.2 Borosilicate volumetric flasks meeting Specification E288 or conforming to ISO 1042, 100mL and 200mL,6.2.1.3 Borosilicate volumetric pipets meeting Specification E969 or piston-operated pipets conforming to ISO 8655, volumeas needed,6.2.1
37、.4 Linear polyethylene bottles with caps, 100mL,6.2.1.5 Analytical balance, accurate to 60.1 mg,6.2.1.6 Glass funnels,E1645 1636.2.1.7 Filter paper, and6.2.1.8 Weighing Paper or Weighing Boat.6.2.2 Apparatus-Microwave Digestion:6.2.2.1 Centrifuge, with 30 mL polysulfone centrifuge tubes and polyprop
38、ylene screw closure,6.2.2.2 Borosilicate volumetric pipets meeting Specification E969 or piston-operated pipets conforming to ISO 8655, volumeas needed,6.2.2.3 Mechanical shaker, and6.2.2.4 Analytical balance, accurate to 60.1 mg.6.2.3 Mortar and pestle (porcelain or agate), shatter box, or mixer mi
39、ll.6.2.4 Plastic gloves, powderless.6.2.5 Thermometers, red alcohol, that cover a range from 0 to 110C.6.3 Reagents, Glassware and Supplies: Reagents:6.2.1 Apparatus-Hot Plate Digestion:6.2.1.1 Borosilicate glass beakers, 125-mL or 50-mL with watchglass covers,6.2.1.2 Class A borosilicate volumetric
40、 flasks, 100mL and 200mL,6.2.1.3 Class A borosilicate volumetric pipets, volume as needed,6.2.1.4 Linear polyethylene bottles with caps, 100mL,6.2.1.5 Analytical balance, accurate to 60.1 mg,6.2.1.6 Glass funnels,6.2.1.7 Filter paper, and6.2.1.8 Weighing Paper or Weighing Boat.6.2.2 Apparatus-Microw
41、ave Digestion:6.2.2.1 Centrifuge, with 30 mL polysulfone centrifuge tubes and polypropylene screw closure,6.2.2.2 Class A volumetric and graduated pipets,6.2.2.3 Mechanical shaker, and6.2.2.4 Analytical balance, accurate to 60.1 mg.6.3.1 Reagents-Hot Plate Digestion:6.3.1.1 Concentrated nitric acid,
42、 ACS reagent grade or spectrographic grade 16.0 M HNO3,6.3.1.2 Nitric acid, 10 % (w/v): Add 100 mL concentrated HNO3 to 500 mL ASTM Type I water (see Specification D1193).Dilute to 1 L with ASTM Type I water,6.3.1.3 Hydrogen peroxide, 30 % H2O2 (w/w); ACS reagent grade, and6.3.1.4 ASTM Type I water
43、(see Specification D1193).6.3.2 Reagents-Microwave Digestion:6.3.2.1 Concentrated nitric acid, ACS reagent grade or spectrographic grade 16.0 M HNO3,6.3.2.2 Concentrated hydrochloric acid, ACS reagent grade 12.3 M HCl,6.3.2.3 ASTM Type I water (see Specification D1193), and6.3.2.4 Extraction Solutio
44、nIn a 1-L volumetric flask, combine the following in order and mix well: 500 mL ASTM Type Iwater, 60 mL concentrated HNO3 and 180 mL concentrated HCl. CoolAllow to cool to room temperature and dilute to 1 L withASTM Type I water. (WarningNitric and hydrochloric acid fumes mists and vapors are toxic.
45、 Prepare in a well-ventilated fumehood.)7. Sample Treatment7.1 Sample Preparation:7.1.1 Sample Mass and AreaAfter analysis, report the final results in area concentration (mg Pb/cm2) or mass concentration(ppm Pb, percent Pb by mass, or alternative units). If area concentration is desired, sample are
46、as must be provided (by the personsubmitting the samples) for each paint sample (chip, powder, etc.). and so forth).The total mass of area concentration samples mustbe determined. Samples may be subsampled (after grinding and homogenization), depending on the sample mass.7.1.2 Area SamplesFor each f
47、ield sample, homogenize the dried paint sample (inside the original sample container, ifpossible) as described in the following:7.1.2.1 Don a new clean pair of vinylplastic gloves to perform sample handling.7.1.2.2 Remove any large amounts of substrate present in the sample. Exercise care when remov
48、ing substrate to avoid any lossesof paint. If required, use a clean safety razor blade or equivalent tool to aid in substrate removal.7.1.2.3 Determination of Total Collected Sample MassAccurate determination of the collected sample mass is required toreport lead analysis results in terms of area co
49、ncentration (mass per unit area of paint sample). A complete transfer of the sampleis required to whatever preweighed container is used to hold the sample during mass determination (for example, weighing boator weighing paper). Total mass shall be made to the nearest 0.1 mg.The following precautions shall be observed during determination of total mass:E1645 164(1) Total sample mass can be determined either before or after sample homogenization. Determination of total sample massis generally advisable prior to homogenization when samp
