ASTM_D_5197_-_21.pdf

Designation:D519721Standard Test Method forDetermination of Formaldehyde and Other CarbonylCompounds in Air(Active Sampler Methodology)1This standard is issued under the fixed designation D5197;the number immediately following the designation 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 presents a procedure for the determi-nation of formaldehyde(HCHO)and other carbonyl com-pounds(aldehydes and ketones)in air.Other carbonyl com-pounds that have been successfully quantified by this methodinclude acetaldehyde,acetone,propanal(propionaldehyde),2-butanone(methylethylketone),butyraldehyde,benzaldehyde,isovaleraldehyde,valeraldehyde,o-tolualdehyde,m-tolualdehyde,p-tolualdehyde,hexanal,and2,5-dimethylbenzaldehyde.1.2 This test method involves drawing air through a car-tridgecontainingsilicagelcoatedwith2,4-dinitrophenylhydrazine(DNPH)reagent.Carbonyl compoundsreadily form stable derivatives with the acidified DNPHreagent.The DNPH derivatives are analyzed for parent alde-hydes and ketones using high performance liquid chromatog-raphy(HPLC)or ultra-high performance liquid chromatogra-phy(UHPLC).UHPLC systems use higher pressures andsmaller particle sizes in columns compared to HPLC systems.The sampling procedure is a modification of U.S.EPA MethodTO-11A(see 2.2).1.3 This test method is based on the reaction of carbonylcompounds with DNPH in the presence of an acid to formstable derivatives according to the reaction shown in Fig.1,(where:both R and R1are alkyl or aromatic groups(ketones),or either,or both R or R1is a hydrogen atom(aldehydes).Thedetermination of formaldehyde and other carbonyl compounds,as DNPH derivatives,is similar to that of U.S.EPA MethodTO-11A in that it uses HPLC or UHPLC for separation ofcarbonyl compounds followed by UV adsorption or photodiodearray detection.This test method exceeds the stated applica-bility of TO-11Ato include other carbonyl compounds that canbe determined as stated in 10.2.4.This test method is suitablefor determination of formaldehyde and other carbonyl com-pounds in the airborne concentration range from approximately10 ppbv/v(12 g/m3),requires sampling for 1 h at 1 L min)to1 ppmv/v(1.2 mg m3).Lower concentrations in air may bedetermined using higher sampling volume and with control ofcontamination,appropriate selection of flow rate and samplingduration.1.4 The sampling method gives a time-weighted average(TWA)sample.It can be used for long-term(1 to 24 h)orshort-term(5 to 60 min)sampling of air for formaldehyde.Shorter sampling times or low flow rates will result in higherdetection limits and may result in greater variation in co-located sampler results.Tests should be performed over aduration and a flow rate that allows the data quality objectiveof the project to be achieved.Sample times for other carbonyls,such as acetaldehyde,may be limited to short term(1).2Thedata provides total concentrations of carbonyl compounds fromwhich time weighted average concentrations can be calculated.1.5 This test method instructs the user on how to preparesampling cartridges from commercially available chromato-graphic grade silica gel cartridges3by the application ofacidified DNPH to each cartridge.1.6 The sampling flow rate,as described in this test method,has been validated for sampling rates up to 1.5 L/min forformaldehyde.This flow rate limitation is principally due to thehigh pressure drop(8 kPa at 1.0 L/min)across user preparedsilica gel cartridges which have a particle size of 55 to 105 m.These cartridges are not generally compatible with battery-powered pumps used in personal sampling equipment(forexample,those used by industrial hygienists).1.7 Alternatively,pre-coated DNPH silica gel cartridges arecommercially available and may be substituted provided theycan be demonstrated to meet blank and analyte trappingacceptance criteria(2).Some of these use silica gel of a largerparticle size that results in a lower pressure drop across thecartridge.These low pressure drop cartridges may be moresuitable for sampling air using battery-powered personal sam-pling pumps.1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.Current edition approved Sept.1,2021.Published May 2022.Originallyapproved in 1991.Last previous edition approved in 2016 as D5197 16.DOI:10.1520/D5197-22.2The boldface numbers in parentheses refer to a list of references at the end ofthis standard.3The cartridge used in the development and performance evaluation of this testmethod was the Sep-Pak Plus Silica cartridge.Other manufactures make similarproducts.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed