AOAC-RI ERP Book - FAOM METHOD.pdf

M ASTOVSKA ET AL .: J OURNAL OF AOAC I NTERNATIONAL V OL . 98, N O . 2, 2015 485

Table 2014.08C. ( continued )

1R RI laboratories

1R RI replicates

Mean concn, μg/kg

Mean recovery, % s r

PAH

, μg/kg s R

, μg/kg RSD r

, % RSD R

, % HorRat

10

20 18 20 16 16 16 16 20 20 20

Naph

9

10

8 8 8 8

Phe

Pyr

10 10 10

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WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR D P/ YROXPHWULF ÀDVN DQG dilute to volume with isooctane. ( e ) Internal standard solution.— 3UHSDUH —J P/ VROXWLRQ RI & 3$+V LQ LVRRFWDQH E\ IROG GLOXWLRQ RI WKH —J P/ (3$ & 3$+V FRFNWDLO ZLWK LVRRFWDQH ( f ) Calibration standard solutions— 3UHSDUH HLJKW OHYHOV RI FDOLEUDWLRQ VWDQGDUG VROXWLRQV P/ HDFK LQ P/ DPEHU VFUHZ FDS YLDOV ,W LV UHFRPPHQGHG WR GLVWULEXWH VPDOO SRUWLRQV HQRXJK IRU D VLQJOH LQMHFWLRQ RI WKH FDOLEUDWLRQ VWDQGDUG VROXWLRQV LQWR PXOWLSOH FULPS WRS YLDOV ZLWK —/ GHDFWLYDWHG JODVV LQVHUWV See Table 2014.08A for analyte concentrations in the calibration standards and Table 2014.08F for the dilution scheme. ( 1 ) For level 1 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 2 ) For level 2 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 3 ) For level 3 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 4 ) For level 4 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ % LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 5 ) For level 5 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 6 ) For level 6 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 7 ) For level 7 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH :RUNLQJ 3$+ 6ROXWLRQ $ LQWR WKH YLDO DQG DGG —/ RI WKH —J P/ & 3$+V VROXWLRQ DQG —/ LVRRFWDQH &DS WKH YLDO DQG YRUWH[ PL[ EULHÀ\ ( 8 ) For level 8 calibration standard ±$FFXUDWHO\ WUDQVIHU —/ RI WKH PL[HG VWRFN VWDQGDUG VROXWLRQ LQWR WKH YLDO DQG

D. Reference Standards

( a ) PAH standards.— +LJK SXULW\ UHIHUHQFH VWDQGDUGV RI WKH 3$+DQDO\WHV GLPHWK\OSKHQDQWKUHQH PHWK\OQDSKWKDOHQH PHWK\OSKHQDQWKUHQH GLPHWK\OQDSKWKDOHQH PHWK\O FKU\VHQH DQWKUDFHQH EHQ]> a @DQWKUDFHQH EHQ]R> a ]pyrene, EHQ]R> b @ÀXRUDQWKHQH EHQ]R> g,h,i @SHU\OHQH EHQ]R> k ] ÀXRUDQWKHQH FKU\VHQH GLEHQ]> a,h @DQWKUDFHQH ÀXRUDQWKHQH ÀXRUHQH LQGHQR> cd ]pyrene, naphthalene, phenanthrene, and pyrene). ( b ) U.S. Environmental Protection Agency (EPA) 16 PAH cocktail.— ( & 3URGXFW 1R (6 —J P/ P/ LQ QRQDQH &DPEULGJH ,VRWRSH /DEV 7HZNVEXU\ 0$ 86$ ) or equivalent. &RQWDLQLQJ $FHQDSKWKHQH & 6 DFHQDSKWK\OHQH ( & 6 DQWKUDFHQH & 6 EHQ]> a ]anthracene ( & 6 , EHQ]R> b @ÀXRUDQWKHQH & 6 EHQ]R> k @ÀXRUDQWKHQH ( & 6 EHQ]R> g,h,i ]perylene ( & 12 EHQ]R> a ]pyrene ( & 4 FKU\VHQH & 6 GLEHQ]> a,h ]anthracene ( & 6 ÀXRUDQWKHQH & 6 ÀXRUHQH & 6 LQGHQR> cd ]pyrene ( & 6 QDSKWKDOHQH & 6 phenanthrene ( & 6 DQG S\UHQH & 6 E. Preparation of Standard Solutions ( a ) Individual stock solutions.— Prepare individual PAH VWRFN VROXWLRQV DW DSSUR[LPDWHO\ RU —J P/ LQ WROXHQH ( b ) Mixed stock standard solution.— 8VH DQDO\WH LQGLYLGXDO stock solutions to obtain a mixed solution of each PAH at —J P/ IRU EHQ]R> a @S\UHQH DQG RWKHU ORZ OHYHO 3$+V RU —J P/ IRU FKU\VHQH DQG RWKHU KLJKHU OHYHO 3$+V RU —J P/ IRU QDSKWKDOHQH LQ LVRRFWDQH See Table 2014.08E for analyte concentrations in the mixed stock standard solution. ( c ) Working PAH Solution A.— $FFXUDWHO\ WUDQVIHU P/ RI WKH PL[HG VWRFN VWDQGDUG VROXWLRQ LQWR D P/ YROXPHWULF ÀDVN and dilute to volume with isooctane. ( d ) Working PAH Solution B.— $FFXUDWHO\ WUDQVIHU P/ RI