This document provides a summary of EPA Method 8082 for analyzing polychlorinated biphenyls (PCBs) in extracts using gas chromatography with an electron capture detector (GC-ECD). Key steps include:
1. Performing an initial 5-point calibration using a mixture of Aroclors 1016 and 1260 to generate calibration factors.
2. Analyzing sample extracts and comparing peaks to the most similar Aroclor standard to quantify PCBs. Identification is based on retention time matches and recognizable Aroclor patterns.
3. Quality control includes an initial calibration verification standard, continuing calibration standards every 20 samples, and a laboratory control sample to verify accuracy and precision.
This document provides a summary of EPA Method 8082 for analyzing polychlorinated biphenyls (PCBs) in extracts using gas chromatography with an electron capture detector (GC-ECD). Key steps include:
1. Performing an initial 5-point calibration using a mixture of Aroclors 1016 and 1260 to generate calibration factors.
2. Analyzing sample extracts and comparing peaks to the most similar Aroclor standard to quantify PCBs. Identification is based on retention time matches and recognizable Aroclor patterns.
3. Quality control includes an initial calibration verification standard, continuing calibration standards every 20 samples, and a laboratory control sample to verify accuracy and precision.
This document provides a summary of EPA Method 8082 for analyzing polychlorinated biphenyls (PCBs) in extracts using gas chromatography with an electron capture detector (GC-ECD). Key steps include:
1. Performing an initial 5-point calibration using a mixture of Aroclors 1016 and 1260 to generate calibration factors.
2. Analyzing sample extracts and comparing peaks to the most similar Aroclor standard to quantify PCBs. Identification is based on retention time matches and recognizable Aroclor patterns.
3. Quality control includes an initial calibration verification standard, continuing calibration standards every 20 samples, and a laboratory control sample to verify accuracy and precision.
Polychlorinated Biphenyls PCBs by Gas Chromatography:
Capillary Column Technique
(EPA Method !"# $!% Description Method 8082 is used to determine PCBs as Aroclors in extracts from a variety of matrices. !ee !"P #$0%0& $020 for preparatory information' (he sample extract is introduced into the )C *y direct in+ection post solvent extraction or dilution. (he )C is temperature pro,rammed to allo- capillary column to separate the compounds& -hich are measured& via an .lectron Capture Detector .CD'. !ystem method sensitivity varies *y matrix. (he estimated /uantitation limits on avera,e are %.0m,01, -et -ei,ht' for soils and oils& and %.0,02 for -aters. A measured volume or -ei,ht one 2iter for li/uids& 23 40,rams for solids' is extracted usin, the appropriate extraction techni/ue. !ample Preservation and Preparation5 !amples to *e analy6ed must *e collected in a ,lass container -ith a (eflon3lined lid. !amples must *e transported and retained under refri,eration at 78C until extraction. !amples may *e held for 9 days prior to extraction and 70 days prior to analysis under refri,eration. :nterferences !ample analysis *y )C re/uires attention to preparatory detail to prevent analytical interference. :nterference can exist as a result of the sample matrix itself or contaminated rea,ents and instrumentation cleanliness. .levated sulfur or parafin re/uires additional cleanup via copper -ash& silica ,el& or ;lorisil. All ,lass-are associated -ith the extraction and concentration processes must *e thorou,hly cleaned& solvent rinsed and oven *a<ed prior to use. :t is found that soaps have *een the source of contamination as -ell as acetone& -hich may *e used durin, cleanup. A ri,orous preventative maintenance routine is mandatory to maintain instrument performance. Apparatus and Materials 3Column5 DB3=& 0.=4mm:D and 0.84m film thic<ness DB3%90%& 0.=4mm:D and 0.84m film thic<ness DB3$08& 0.=4mm :D x 40M len,th 3)as Chromato,raph5 >P =8?0 !eries ::& Dual Detector !ystem >P =8?0A 3Data !ystem5 >P Chemstation %90%B Procedure $9%0 @evised 04009 % @ea,ents and !tandards 3!tandards are purchased as certified solutions 3"r,anic ;ree rea,ent -ater 3All solvent lots used are pesticide /uality or e/uivalent and should *e phthalate free. 3!urro,ate !tandards3 Decachloro*iphenyl and (etrachloro3m3xylene mix is used as surro,ate and is added to each sample prior to extraction 3Cali*ration !tandards for Aroclors5 A multi3point initial cali*ration employin, a mixture of Aroclor %0%$ and %2$0 in e/ual ratio at five concentrations& is used to demonstrate the linearity of the detector response. "ther Aroclors need to *e run at -or<in, ran,e of the detector to calculate @; and for sample identification. !ee (a*le :: for standard preparation. . 3Matrix !pi<e !tandard5 Aroclor %0%$0%2$0 mixture is used for matrix spi<e in most of the samples *ut -hen a particular Aroclor is expected in samples the specific Aroclor should *e used for spi<in,. 32a*oratory Control !ample 2C!'. Aroclor %0%$0%2$0 mixture is used for 2C! Aote5 All standards are stored at B%08C to B208C in am*er *ottles -ith (eflon3 lined scre- caps. All stoc< standards are sta*le for one year. Procedure 1.0 Initial Calibration %.% Perform re/uired preventative maintenance includin, evaluatin, the auto36ero num*er for saturation of the .CD detector& -hich should *e less than %= and should not vary more than %.0 from the previous days run. %.2 An initial five3point cali*ration is performed usin, mixture of Aroclors %0%$0%2$0. (he concentration should correspond to the expected ran,e of concentrations found in real samples and should *rac<et the linear ran,e of the detector. !ee (a*le :: for concentration of analytes at cali*ration level. %.4 !tandards of the other five Aroclors are run for pattern reco,nition and also to determine sin,le point cali*ration for each Aroclor. Procedure $9%0 @evised 04009 2 %.7 )C operatin, conditions are esta*lished for proper resolution and sensitivity. !ee (a*le : for )C conditions. (he same operatin, conditions are to *e used for *oth cali*rations and sample analysis. %.= 22 of in+ection enters the ,uard column. (he splitter then simultaneously in+ects on *oth column and detector systems. ;or a sin,le channel detector&%ul is in+ected onto the column. %.$ A minimum of five pea<s are chosen for identification purposes. "ne of the chosen pea<s must *e that uni/ue to the Aroclor. Also at least five pea<s for the Aroclor %0%$0%020 mixture& none of -hich should *e found in *oth of these Aroclors. %.9 !ee (a*le ::: for dia,nostic pea<s in each Aroclor alon, -ith their retention times @('. %.8 Cali*ration factor C;' is calculated as ,iven *elo- on the five3point cali*ration !(D as ,iven in %.2. C; C Pea< area in the !(D'0(otal mass of !(D in+ected n,' ;ive sets of C; -ill *e ,enerated for the Aroclor %0%$0%2$0 mixture& each set consistin, of the C; for each of the five pea<s chosen for the mixture. (his data is used to determine mean C;& standard deviation !D' and relative standard deviation @!D'. Percent @!D should *e less than 20D for linear response. %.? @etention time -indo-s5 :n+ect mixture of %0%$0%2$0 three times over a period of 92 hours calculate mean and !(D deviation of at least five chosen pea<s. (he -idth of the retention time -indo- for each analyte& surro,ate and ma+or constituent in multi3component analytes is defined as E03 4 times the !D of the mean a*solute retention esta*lished durin, the 923hour period. (a*le :F lists a summary of retention times of Aroclors. %.%0 @etention times of the surro,ate should *e monitored more closely. Ghenever the o*served retention time of the surro,ate is outside of the esta*lished retention time -indo-& the cause of the pro*lem *e determined and corrective action ta<en *efore continuin, analyses. 2.0 GC Analysis of sample extract 2.% Mix of %0%$0%2$0 is used as cali*ration chec< !(D. (he C; for each analyte calculated from the cali*ration verification standard C; v ' must not exceed a difference of more than E03 %=D -hen compared to the mean C; from the initial cali*ration curve. Procedure $9%0 @evised 04009 4 D Difference C HC;3C;v'0C;I J %00 D Difference should *e K %=D 2.2 Ferify cali*ration each %23hour shift. A cali*ration !(D must also *e in+ected at intervals of not less than once every 20 samples and at the end of the analysis se/uence. 2.4 :f the D difference exceeds %=D& inspect the ,as chromato,raphy system to determine the cause and perform -hatever maintenance is necessary. :f reanalysis of cali*ration verification !(D fails& a ne- initial cali*ration must *e performed. 2.7 :f the pea< response is less than 2.= times the *aseline noise level the validity of the /uantitative results may *e /uestiona*le. Cali*ration !(D should also *e used to evaluate retention time sta*ility. 3.0 Qualitative Analysis 4.% (he identification of PCBs is *ased on retention time match and also *ased on a clearly identifia*le Aroclor pattern. Positive PCB must *e verified *y a second column confirmation. Ghen samples are analy6ed from a source <no-n to contain specific Aroclors& the results from a sin,le3column analysis may *e confirmed on the *asis of a clearly reco,ni6a*le Aroclor pattern. 4.0 Quantitation of PC!s as Aroclor 7.% (he Luantitation of PCB residues as Aroclors is accomplished *y comparison of the sample chromato,ram to that of the most similar Aroclor standard. Compare the response of at least five ma+or pea<s in the sin,le point cali*ration standard for that Aroclor -ith the pea<s o*served in the sample extract. (he amount of Aroclor is calculated usin, the individual cali*ration factor for each pea< selected. (he concentration is determined *y avera,in, the concentration of all selected pea<s. 7.%.% Geatherin, of PCBs in the environment and chan,es resultin, from -aste treatment processes may alter the PCBs to the point that the pattern of a specific Aroclor is no lon,er reco,ni6a*le. !amples also containin, more than one Aroclor present similar pro*lems. Ghen /uantitation and identification is done in these types of situation& the pro*lem is documented and descri*ed to the data user. Procedure $9%0 @evised 04009 7 Luality Control :nitial demonstration of proficiency is demonstrated *y ,eneratin, data of accepta*le accuracy and precision for tar,et analytes in a clean matrix. LC reference sampleM %0m,02 mixture of %0%$0%2$0 is used as LC reference sample. %m2 of this standard is spi<ed into %2 of or,anic free rea,ent -ater. >o-ever& -hen specific Aroclors are <no-n to *e present of expected in samples& the specific Aroclors are used for the LC reference sample. LC reference sample is analy6ed % per 20 samples or % per *atch if less than 20 samples. Accepta*le recovery limit is 803%20D. Cali*ration !(D should *e run every 20 samples. (he cali*ration factors for the cali*ration should *e -ithin %=D of the initial cali*ration chec<. Matrix spi<e& matrix spi<e duplicateM %0m,02 mixture is used for matrix spi<e and spi<e duplicate. >o-ever& -hen specific Aroclors are <no-n to *e present or expected in samples& the specific Aroclors should *e used for spi<in,. A la*oratory control sample 2C!'. 2C! is spi<ed -ith matrix spi<e standard %0%$0%2$0 in clean matrix. !urro,ate recoveriesM !urro,ate recovery data from individual samples is compared -ith the surro,ate control limits developed *y the la*oratories. ;ailure to meet /uality control accepta*le limits re/uires corrective action see procedure 0%=0'. 2ocate and correct the source of the pro*lem and repeat the test. ;ailure to meet /uality control accepta*le limits a,ain -ill re/uire ne- cali*ration curve. @eferences5 !G 87$ Method 8082 pp. 80823% to 808237% @evision 0 Decem*er %??$ Procedure $9%0 @evised 04009 = Procedure $9%0 @evised 04009 $ Gide *ore column Column flo- =39 m20 minute Carrier ,as0ma<e3up ,as A2 ??.?????D' :n+ector (emperature 2=08C Detector (emperature 4=08C :nitial oven (emperature (emperature rate 70 minutes ;inal (emperature (otal Pro,ram (ime 7% minutes (a*le : GC "peratin# Con$itions for PC%s as Aroclors 40x0.=4mm:Dx0.84mm film DB%90% 40x0.=4mm:Dx0.84mm film DB= %=08C hold for = minutes 29=8C hold for = minutes !(D #% 2.= 20 =00 % !(D #2 2.= =0 =00 2 !(D #4 2.= %00 =00 = !(D #7 2.= %=0 =00 %0 !(D #= 2.= 200 =00 20 !(D Conc.,0m2' (a*le :: Calibration &tan$ar$ Preparation NN:ndividual cali*ration standards are re/uired for each Aroclor.NN. %0%$0%2$0 Aroclors !toc< Conc. ,0m2' Folume !toc< !olution ,0m2' ;inal Folume ,0m2' Procedure $9%0 @evised 04009 9 Pea< Ao. @( on DB3$08 Aroclor % 9.$8 %22%& %242 2 8.82 %22%& %242 4 %0.4= %22%& %242& %0%$ 7 %0.?7 %22%& %242& %0%$ = %%.2 %0%$& %22%& %242& %272 $ %%.7$ %22%& %0%$& %242 9 %2.84 %0%$& %242& %272& %278 8 %7.22 %0%$& %242& %272& %278 ? %7.89 %242& %0%$& %272& %278 %0 %=.4? %242& %0%$& %272 %% %=.79 %278& %2=7 %2 %$.$? %242& %0%$& %272 %4 %9.%$ %242& %0%$& %272& %278 %7 %9.$8 %2=7& %278& %272 %= %9.?% %0%$& %242& %272 %$ %9.?4 %278& %2=7& %272 %9 %8.24 %2=7& %2$0& %278 %8 %8.7= %2=7& %2$0& %278 %? %8.?8 %278& %272& %242& %2=7 20 20 %2=7& %2$0& %278& %272 2% 20.7% %2=7& %272& %278 22 20.84 %2=7& %278 24 2%.0= %2$0& %2=7 27 2%.47 %2=7& %2$0 2= 22.0? %2$0& %2=7 2$ 22.7% %272& %278& %2=7 29 22.$% %2$0& %2=7 28 22.?9 %2=7& %2$0 2? 27.$? %2$0 40 2=.47 %2$0& %2=7 4% 28.04 %2$0& %2=7 Pea<s are se/uentially num*ered in elution order and are not isomer num*er Onderline indicates lar,est pea< in the pattern for that Aroclor Pea's (ia#nostic of PC%s observe$ on 0.)3mm I( Column $urin# sin#le column analysis ;or comparison use only (a*le ::: Procedure $9%0 @evised 04009 8 Pea< Ao. %0%$ %22% %242 %272 %278 %2=7 %2$0 % 9.$8 9.$8 2 8.82 8.82 4 %0.4= %0.4= %0.4= 7 %0.?7 %0.?7 %0.?7 = %%.20 %%.20 %%.20 %%.20 $ %%.7$ %%.7$ %%.7$ %%.7$ 9 %2.84 %2.84 %2.84 %2.84 8 %7.22 %7.22 %7.22 %7.22 %7.22 ? %7.89 %7.89 %7.89 %7.89 %0 %=.4? %=.4? %=.4? %2 %=.79 %=.79 %4 %$.$? %$.$? %$.$? %7 %9.%$ %9.%$ %9.%$ %9.%$ %= %9.$8 %9.$8 %9.$8 %$ %9.%? %9.?% %9.?% %9 %9.?4 %9.?4 %9.?4 %8 %8.24 %8.24 %8.24 %? %8.7= %8.7= %8.7= 20 %8.?8 %8.?8 %8.?8 %8.?8 2% 20.7% 20.7% 20.7% 22 20.84 20.84 24 2%.0= 2%.0= 27 2%.47 2%.47 2= 22.7% 22.7% 22.7% 2$ 22.$% 22.$% 29 22.?9 22.?9 28 27.$? 2? 2=.47 2=.47 40 28.04 28.04 (a*le :F &ummary of *etention +imes of Aroclors or (,-0. Procedure $9%0 @evised 04009 ?
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