Initial hold time (minutes)..........  2......................  2......................  2.
Temperature program..................  100 to 190 [deg]C at 40  100 to 300 [deg]C at     100 to 150 [deg]C at 15
                                        [deg]C/min, then 190     8[deg]C/min.             [deg]C/min, then 150
                                        to 300 [deg]C at                                  to 290 [deg]C at 2.5
                                        3[deg]C/min.                                      [deg]C/min.
----------------------------------------------------------------------------------------------------------------

             Table 23-17--Assignment of Pre-Extraction Standards for Quantitation of Target PCB \b\
----------------------------------------------------------------------------------------------------------------
                PCB Congener                    BZ No.\a\               Labeled analog                BZ No.
----------------------------------------------------------------------------------------------------------------
2,4'-DiCB (NOAAT)..........................               8  \13\C12-2,2'-DiCB..................              4L
2,2',5-TrCB (NOAAT)........................              18  \13\C12-2,2',6-TrCB................             19L
2,4,4'-TrCB (NOAAT)........................              28  \13\C12-2,2',6-TrCB................             19L
2,2',3,5'-TeCB (NOAAT).....................              52  \13\C12-2,2',6,6'-TeCB.............             54L
2,2',5,5'-TeCB (NOAAT).....................              52  \13\C12-2,2',6,6'-TeCB.............             54L
2,3',4,4'-TeCB (NOAAT).....................              66  \13\C12-2,2',6,6'-TeCB.............             54L
3,3',4,4'-TeCB (NOAAT) (WHOT)..............              77  \13\C12-3,3',4,4'-TeCB.............             77L
3,4,4',5-TeCB (WHOT).......................              81  \13\C12-3,4,4'',5-TeCB.............             81L
2,2',4,5,5'-PeCB (NOAAT)...................             101  \13\C12-2,2',4,5,5'-PeCB...........            104L
2,3,3',4,4'-PeCB (NOAAT) (WHOT)............             105  \13\C12-2,3,3',4,4'-PeCB...........            105L
2,3,4,4',5-PeCB (WHOT).....................             114  \13\C12-2,3,4,4',5-PeCB............            114L
2,3',4,4',5-PeCB (WHOT)....................             118  \13\C12-2,3',4,4',5-PeCB...........            118L
2',3,4,4',5-PeCB (WHOT)....................             123  \13\C12-2',3,4,4',5-PeCB...........            123L
3,3',4,4',5-PeCB (NOAAT) (WHOT)............             126  \13\C12-3,3',4,4',5-PeCB...........            126L
2,2',3,3',4,4'-HxCB (NOAAT)................             128  \13\C12-2,2',4,4',6,6'-HxCB........            155L
2,2',3,4,4',5'-HxCB (NOAAT)................             138  \13\C12-2,2',4,4',6,6'-HxCB........            155L
2,2',4,4',5,5'-HxCB (NOAAT)................             153  \13\C12-2,2',4,4',6,6'-HxCB........            155L
2,3,3',4,4',5-HxCB (WHOT)..................             156  \13\C12-2,3,3',4,4',5-HxCB.........            156L
2,3,3',4,4',5'-HxCB (WHOT).................             157  \13\C12-2,3,3',4,4',5'-HxCB........            157L
2,3',4,4',5,5'-HxCB (WHOT).................             167  \13\C12-2,3',4,4',5,5'-HxCB........            167L
3,3',4,4',5,5'-HxCB (NOAAT) (WHOT).........             169  \13\C12-3,3',4,4',5,5'-HxCB........            169L
2,2',3,3',4,4',5-HpCB (NOAAT)..............             170  \13\C12-2,2',3,3',4,4',5'-HpCB.....            170L
2,2',3,4,4',5,5'-HpCB (NOAAT)..............             180  \13\C12-2,2',3,4,4',5,5'-HpCB......            180L
2,2',3,4',5,5',6-HpCB (NOAAT)..............             187  \13\C12-2,2',3,4',5,6,6'-HpCB......            188L
2,3,3',4,4',5,5'-HpCB (WHOT)...............             189  \13\C12-2,3,3',4,4',5,5'-HpCB......            189L

2,2',3,3',4,4',5,6-OcCB (NOAAT)............             195  \13\C12-2,2' 3,3',5,5',6,6'-OcCB...            202L
2,2',3,3',4,4',5,5',6-NoCB (NOAAT).........             206  \13\C12-2,2',3,3',4,4',5,5',6-NoCB.            206L
2,2',3,3',4,4',5,5',6,6'-DeCB (NOAAT)......             209  \13\C12-DeCB.......................            209L
----------------------------------------------------------------------------------------------------------------
\a\ BZ No.: Ballschmiter and Zell 1980, or IUPAC number.
\b\ Assignments assume the use of the SPB-Octyl column. In the event you choose another column, you may select
  the labeled standard having the same number of chlorine substituents and the closest retention time to the
  target analyte in question as the labeled standard to use for quantitation.
NOAAT = PCB considered toxic by the National Oceanic and Atmospheric Administration.
WHOT = PCB considered toxic by the World Health Organization.

                        Table 23-18--Initial Demonstration of Capability QC Requirements
----------------------------------------------------------------------------------------------------------------
                                                                  Specification and
             Section                      Requirement                 frequency            Acceptance criteria
----------------------------------------------------------------------------------------------------------------
9.3.5............................  Demonstration of low       Analyze an LMB after the  Confirm that the LMB is
                                    system background.         highest calibration       free from contamination
                                                               standard.                 as defined in Section
                                                              Note: If an automated      13.1.
                                                               extraction system is
                                                               used, an LMB must be
                                                               extracted on each port.
9.3.7............................  Determination of MDL.....  Prepare, extract, and     See MDL confirmation.
                                                               analyze 7 replicate
                                                               spiked samples (spiked
                                                               within 2 to 10 times of
                                                               the expected MDL) and 7
                                                               LMBs.
                                                              See 40 CFR Part 136
                                                               Appendix B.
9.3.8............................  MDL confirmation.........  Prepare, extract, and     Confirm that the target
                                                               analyze a spiked sample   compounds meet the
                                                               (spiked at the MDL).      qualitative
                                                                                identification criteria
                                                                                in Section <IP_ADDRESS> of
                                                                                this method.
9.3.9............................  Demonstration of           Prepare, extract, and     Percent relative
                                    precision.                 analyze 7 replicate       standard deviation must
                                                               spiked samples (spiked    be <=20%.
                                                               near mid-range).
9.3.10...........................  Demonstration of accuracy  Calculate mean recovery   Mean recovery within 70-
                                                               for replicate spiked      130% of true value.
                                                               samples in Section
                                                               9.3.9.
9.3.2............................  Lowest Calibration         Establish a target        Upper PIR <=150%.
                                    Concentration              concentration for the    Lower PIR >=50%.
                                    Confirmation.              lowest calibration
                                                               based on the intended
                                                               use of the method.
9.3.6............................  Calibration Verification.  Analyze a mid-level QCS.  Within limits in Section
                                                                                13.11.
----------------------------------------------------------------------------------------------------------------

[GRAPHIC] [TIFF OMITTED] TR20MR23.019

Figure 23-1. Method 23 Sampling Train

[GRAPHIC] [TIFF OMITTED] TR20MR23.020

Figure 23-2. Condenser and Adsorbent Module

[GRAPHIC] [TIFF OMITTED] TR20MR23.021

Figure 23-3. Soxhlet/Dean-Stark Extractor

[GRAPHIC] [TIFF OMITTED] TR20MR23.022

Figure 23-4. Sample Preparation Flow Chart

Appendix A to Method 23

                   Complete List of 209 PCB Congeners and Their Isomers With Corresponding Isotope Dilution Quantitation Standards \a\
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                   Unlabeled target                    Pre-extraction                    Unlabeled target
      Pre-extraction standard        BZ \b\ No.         analyte         BZ \b\ No.        standard         BZ \b\ No.         analyte         BZ \b\ No.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                       MoCB                         DiCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2-MoCB....................           1L  2-MoCB..............            1  \13\C12-2,2'-DiCB...           4L  2,2'-DiCB...........            4
\13\C12-2-MoCB....................           1L  3-MoCB..............            2  \13\C12-2,2'-DiCB...           4L  2,3-DiCB............            5
\13\C12-4-MoCB....................           3L  4-MoCB..............            3  \13\C12-2,2'-DiCB...           4L  2,3'-DiCB...........            6
                                                                                \13\C12-2,2'-DiCB...           4L  2,4-DiCB............            7
                                                                                \13\C12-2,2'-DiCB...           4L  2,4'-DiCB...........            8
                                                                                \13\C12-2,2'-DiCB...           4L  2,5-DiCB............            9
                                                                                \13\C12-2,2'-DiCB...           4L  2,6-DiCB............           10
                                                                                \13\C12-2,2'-DiCB...           4L  3,3'-DiCB...........           11
                                                                                \13\C12-2,2'-DiCB...           4L  3,4-DiCB............           12
                                                                                \13\C12-2,2'-DiCB...           4L  3,4'-DiCB...........           13
                                                                                \13\C12-2,2'-DiCB...           4L  3,5-DiCB............           14
                                                                                \13\C12-4,4'-DiCB...          15L  4,4'-DiCB...........           15
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                          TrCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',6-TrCB...............          19L  2,2',3-TrCB.........           16  \13\C12-3,4,4'-TrCB.          19L  2,4,4'-TrCB.........           28
\13\C12-2,2',6-TrCB...............          19L  2,2',4-TrCB.........           17  \13\C12-3,4,4'-TrCB.          19L  2,4,5-TrCB..........           29
\13\C12-2,2',6-TrCB...............          19L  2,2',5-TrCB.........           18  \13\C12-3,4,4'-TrCB.          19L  2,4,6-TrCB..........           30
\13\C12-2,2',6-TrCB...............          19L  2,2',6-TrCB.........           19  \13\C12-3,4,4'-TrCB.          19L  2,4',5-TrCB.........           31
\13\C12-2,2',6-TrCB...............          19L  2,3,3'-TrCB.........           20  \13\C12-3,4,4'-TrCB.          19L  2,4',6-TrCB.........           32
\13\C12-2,2',6-TrCB...............          19L  2,3,4-TrCB..........           21  \13\C12-3,4,4'-TrCB.          19L  2',3,4-TrCB.........           33
\13\C12-2,2',6-TrCB...............          19L  2,3,4'-TrCB.........           22  \13\C12-3,4,4'-TrCB.          19L  2',3,5-TrCB.........           34
\13\C12-2,2',6-TrCB...............          19L  2,3,5- TrCB.........           23  \13\C12-3,4,4'-TrCB.          19L  3,3',4-TrCB.........           35
\13\C12-2,2',6-TrCB...............          19L  2,3,6- TrCB.........           23  \13\C12-3,4,4'-TrCB.          19L  3,3',5-TrCB.........           36
\13\C12-2,2',6-TrCB...............          19L  2,3',4-TrCB.........           25  \13\C12-3,4',4'-TrCB          37L  3,4,4'-TrCB.........           37
\13\C12-2,2',6-TrCB...............          19L  2,3',5-TrCB.........           26  \13\C12-3,4',4'-TrCB          37L  3,4,5-TrCB..........           38
\13\C12-2,2',6-TrCB...............          19L  2,3',6-TrCB.........           27  \13\C12-3,4',4'-TrCB          37L  3,4',5-TrCB.........           39
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                          TeCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,3'-TeCB......           40  \13\C12-2,2',6,6'-            54L  2,3,4,5-TeCB........           61
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,4-TeCB.......           41  \13\C12-2,2',6,6'-            54L  2,3,4,6-TeCB........           62
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,4'-TeCB......           42  \13\C12-2,2',6,6'-            54L  2,3,4',5-TeCB.......           63
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,5-TeCB.......           43  \13\C12-2,2',6,6'-            54L  2,3,4',6-TeCB.......           64
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,5'-TeCB......           44  \13\C12-2,2',6,6'-            54L  2,3,5,6-TeCB........           65
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,6-TeCB.......           45  \13\C12-2,2',6,6'-            54L  2,3',4,4'-TeCB......           66
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',3,6'-TeCB......           46  \13\C12-2,2',6,6'-            54L  2,3',4,5-TeCB.......           67
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',4,4'-TeCB......           47  \13\C12-2,2',6,6'-            54L  2,3',4,5'-TeCB......           68
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',4,5-TeCB.......           48  \13\C12-2,2',6,6'-            54L  2,3',4,6-TeCB.......           69
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',4,5'-TeCB......           49  \13\C12-2,2',6,6'-            54L  2,3',4',5-TeCB......           70
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',4,6-TeCB.......           50  \13\C12-2,2',6,6'-            54L  2,3',4',6-TeCB......           71
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',4,6'-TeCB......           51  \13\C12-2,2',6,6'-            54L  2,3',5,5'-TeCB......           72
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',5,5'-TeCB......           52  \13\C12-2,2',6,6'-            54L  2,3',5',6-TeCB......           73
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',5,6'-TeCB......           53  \13\C12-2,2',6,6'-            54L  2,4,4',5-TeCB.......           74
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,2',6,6'-TeCB......           54  \13\C12-2,2',6,6'-            54L  2,4,4',6-TeCB.......           75
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,3',4'-TeCB......           55  \13\C12-2,2',6,6'-            54L  2',3,4,5-TeCB.......           76
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,3',4'-TeCB......           56  \13\C12-3,3',4,4'-            77L  3,3',4,4'-TeCB......           77
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,3',5-TeCB.......           57  \13\C12-3,3',4,4'-            77L  3,3',4,5-TeCB.......           78
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,3',5'-TeCB......           58  \13\C12-3,3',4,4'-            77L  3,3',4,5'-TeCB......           79
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,3',6-TeCB.......           59  \13\C12-3,3',4,4'-            77L  3,3',5,5'-TeCB......           80
                                                                                TeCB.
\13\C12-2,2',6,6'-TeCB............          54L  2,3,4,4'-TeCB.......           60  \13\C12-3,4,4',5-             81L  3,4,4',5-TeCB.......           81
                                                                                TeCB.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                          PeCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,3',4-PeCB....           82  \13\C12-2,3,3',4,4'-         105L  2,3,3',4,4'-PeCB....          105
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,3',5-PeCB....           83  \13\C12-2,3,3',4,4'-         105L  2,3,3',4,5-PeCB.....          106
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,3',6-PeCB....           84  \13\C12-2,3,3',4,4'-         105L  2,3,3',4',5-PeCB....          107
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4,4'-PeCB....           85  \13\C12-2,3,3',4,4'-         105L  2,3,3',4,5'-PeCB....          108
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4,5-PeCB.....           86  \13\C12-2,3,3',4,4'-         105L  2,3,3',4,6-PeCB.....          109
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4,5'-PeCB....           87  \13\C12-2,3,3',4,4'-         105L  2,3,3',4',6-PeCB....          110
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4,6-PeCB.....           88  \13\C12-2,3,3',4,4'-         105L  2,3,3',5,5'-PeCB....          111
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4,6'-PeCB....           89  \13\C12-2,3,3',4,4'-         105L  2,3,3',5,6-PeCB.....          112
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4',5-PeCB....           90  \13\C12-2,3,3',4,4'-         105L  2,3,3',5',6-PeCB....          113
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,4',6-PeCB....           91  \13\C12-2,3,4,4',5-          114L  2,3,4,4',5-PeCB.....          114
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,5,5'-PeCB....           92  \13\C12-2,3,4,4',5-          114L  2,3,4,4',6-PeCB.....          115
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,5,6-PeCB.....           93  \13\C12-2,3,4,4',5-          114L  2,3,4,5,6-PeCB......          116
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,5,6'-PeCB....           94  \13\C12-2,3,4,4',5-          114L  2,3,4',5,6-PeCB.....          117
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,5',6-PeCB....           95  \13\C12-2,3',4,4',5-         118L  2,3',4,4',5-PeCB....          118
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3,6,6'-PeCB....           96  \13\C12-2,3',4,4',5-         118L  2,3',4,4',6-PeCB....          119
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3',4,5-PeCB....           97  \13\C12-2,3',4,4',5-         118L  2,3',4,5,5'-PeCB....          120
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',3',4,6-PeCB....           98  \13\C12-2,3',4,4',5-         118L  2,3',4,5,'6-PeCB....          121
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,4',5-PeCB....           99  \13\C12-2,3',4,4',5-         118L  2',3,3',4,5-PeCB....          122
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,4',6-PeCB....          100  \13\C12-2',3,4,4',5-         123L  2',3,4,4',5-PeCB....          123
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,5,5'-PeCB....          101  \13\C12-2',3,4,4',5-         123L  2',3,4,5,5'-PeCB....          124
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,5,6'-PeCB....          102  \13\C12-2',3,4,4',5-         123L  2',3,4,5,6'-PeCB....          125
                                                                                PeCB.
\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,5,'6-PeCB....          103  \13\C12-3,3',4,4',5-         126L  3,3',4,4',5-PeCB....          126
                                                                                PeCB.

\13\C12-2,2',4,6,6'-PeCB..........         104L  2,2',4,6,6'-PeCB....          104  \13\C12-3,3',4,4',5-         126L  3,3',4,5,5'-PeCB....          127
                                                                                PeCB.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                          HxCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',4,4'-HxCB.          128  \13\C12-                     155L  2,2',3,4',5',6-HxCB.          149
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',4,5-HxCB..          129  \13\C12-                     155L  2,2',3,4',6,6'-HxCB.          150
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',4,5'-HxCB.          130  \13\C12-                     155L  2,2',3,5,5',6-HxCB..          151
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',4,6-HxCB..          131  \13\C12-                     155L  2,2',3,5,6,6'-HxCB..          152
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',4,6'-HxCB.          132  \13\C12-                     155L  2,2',4,4',5,5'-HxCB.          153
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',5,5'-HxCB.          133  \13\C12-                     155L  2,2',4,4',5',6-HxCB.          154
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',5,6-HxCB..          134  \13\C12-                     155L  2,2',4,4',6,6'-HxCB.          155
                                                                                2,2',4,4',6,6'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',5,6'-HxCB.          135  \13\C12-                     156L  2,3,3',4,4',5-HxCB..          156
                                                                                2,3,3',4,4',5- HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,3',6,6'-HxCB.          136  \13\C12-                     157L  2,3,3',4,4',5'-HxCB.          157
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,4',5-HxCB..          137  \13\C12-                     157L  2,3,3',4,4',6-HxCB..          158
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,4',5'-HxCB.          138  \13\C12-                     157L  2,3,3',4,5,5'-HxCB..          158
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,4',6-HxCB..          139  \13\C12-                     157L  2,3,3',4,5,6-HxCB...          160
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,4',6'-HxCB.          140  \13\C12-                     157L  2,3,3',4,5',6-HxCB..          161
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,5,5'-HxCB..          141  \13\C12-                     157L  2,3,3',4',5,5'-HxCB.          162
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,5,6-HxCB...          142  \13\C12-                     157L  2,3,3',4',5,6-HxCB..          163
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,5,6'-HxCB..          143  \13\C12-                     157L  2,3,3',4',5',6-HxCB.          164
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,5',6-HxCB..          144  \13\C12-                     157L  2,3,3',5,5',6-HxCB..          165
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4,6,6'-HxCB..          145  \13\C12-                     157L  2,3,4,4',5,6-HxCB...          166
                                                                                2,3,3',4,4',5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4',5,5'-HxCB.          146  \13\C12-                     167L  2,3',4,4',5,5'-HxCB.          167
                                                                                2,3',4,4',5,5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4',5,6-HxCB..          147  \13\C12-                     167L  2,3',4,4',5',6-HxCB.          168
                                                                                2,3',4,4',5,5'-HxCB.
\13\C12-2,2',4,4',6,6'-HxCB.......         155L  2,2',3,4',5,6'-HxCB.          148  \13\C12-                     169L  3,3',4,4',5,5'-HxCB.          169
                                                                                3,3',4,4',5,5'-HxCB.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                          HpCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,4',5-             170  \13\C12-                     188L  2,2',3,4,4',5,6'-             182
                                                  HpCB.                              2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,4',6-             171  \13\C12-                     188L  2,2',3,4,4',5',6-             183
                                                  HpCB.                              2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,5,5'-             172  \13\C12-                     188L  2,2',3,4,4',5',6-             184
                                                  HpCB.                              2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,5,6-HpCB          173  \13\C12-                     188L  2,2',3,4,4',6,6'-             185
                                                                                2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,5,6'-             174  \13\C12-                     188L  2,2',3,4,5,5',6-HpCB          186
                                                  HpCB.                              2,2',3,4',5,6,6'-
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,5',6-             175  \13\C12-                     188L  2,2',3,4',5,5',6-             187
                                                  HpCB.                              2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4,6,6'-             176  \13\C12-                     188L  2,2',3,4',5,6,6'-             188
                                                  HpCB.                              2,2',3,4',5,6,6'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',4',5,6-             177  \13\C12-                     189L  2,3,3',4,4',5,5'-             189
                                                  HpCB.                              2,3,3',4,4',5,5'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',5,5',6-             178  \13\C12-                     189L  2,3,3',4,4',5,6-HpCB          190
                                                  HpCB.                              2,3,3',4,4',5,5'-
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,3',5,6,6'-             179  \13\C12-                     189L  2,3,3',4,4',5',6-             191
                                                  HpCB.                              2,3,3',4,4',5,5'-                  HpCB.
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,4,4',5,5'-             180  \13\C12-                     189L  2,3,3',4,5,5',6-HpCB          192
                                                  HpCB.                              2,3,3',4,4',5,5'-
                                                                                HpCB.
\13\C12-2,2',3,4',5,6,6'-HpCB.....         188L  2,2',3,4,4',5,6-HpCB          181  \13\C12-                     189L  2,3,3',4',5,5',6-             193
                                                                                2,3,3',4,4',5,5'-                  HpCB.
                                                                                HpCB.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                       OcCB                         NoCB
--------------------------------------------------------------------------------------------------------------------------------------------------------
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,4',5,5'-          194  \13\C12-                     206L  2,2',3,3',4,4',5,5',          206
                                                  OcCB.                              2,2',3,3',4,4',5,5'                6-NoCB.
                                                                                ,6-NoCB.

\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,4',5,6-           195  \13\C12-                     206L  2,2',3,3',4,4',5,6,6          207
                                                  OcCB.                              2,2',3,3',4,4',5,5'                '-NoCB.
                                                                                ,6-NoCB.
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,4',5,6'-          196  \13\C12-                     208L  2,2',3,3',4,5,5',6,6          208
                                                  OcCB.                              2,2',3,3',4,5,5',6,                '- NoCB.
                                                                                6'-NoCB.
                                                                                ---------------------------------------------------------------------
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,4',6,6'-          197                                  DeCB
                                                  OcCB.
                                                                                ---------------------------------------------------------------------
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,5,5',6-           198  \13\C12-DeCB........         209L  2,2',3,3',4,4',5,5',          209
                                                  OcCB.                                                                 6,6'-DeCB.
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,5,5',6'-          199
                                                  OcCB.
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,5,6,6'-           200
                                                  OcCB.
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',4,5',6,6'-          201
                                                  OcCB.
\13\C12-2,2',3,3',5,5',6,6'-OcCB..         202L  2,2',3,3',5,5',6,6'-          202
                                                  OcCB.
\13\C12-2,3',3',4,4',5,5',6-OcCB..         205L  2,2',3,4,4',5,5',6-           203
                                                  OcCB.
\13\C12-2,3',3',4,4',5,5',6-OcCB..         205L  2,2',3,4,4',5,6,6'-           204
                                                  OcCB.
\13\C12-2,3',3',4,4',5,5',6-OcCB..         205L  2,3,3',4,4',5,5',6-           205
                                                  OcCB.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ Assignments assume the use of the SPB-Octyl column. In the event you choose another column, you may select the labeled standard having the same
  number of chlorine substituents and the closest retention time to the target analyte in question as the labeled standard to use for quantitation.
\b\ BZ No.: Ballschmiter and Zell 1980, also referred to as IUPAC number.

Appendix B to Method 23

Preparation of XAD-2 Adsorbent Resin

1.0 Scope and Application

    XAD-2[supreg] resin, as supplied by the original manufacturer,
is impregnated with a bicarbonate solution to inhibit microbial
growth during storage. Remove both the salt solution and any
residual extractable chemicals used in the polymerization process
before use. Prepare the resin by a series of water and organic
extractions, followed by careful drying.

2.0 Extraction

    2.1 You may perform the extraction using a Soxhlet extractor or
other apparatus that generates resin meeting the requirements in
Section 13.1 of Method 23. Use an all-glass thimble containing an
extra-coarse frit for extraction of the resin. The frit is recessed
10-15 mm above a crenellated ring at the bottom of the thimble to
facilitate drainage. Because the resin floats on methylene chloride,
carefully retain the resin in the extractor cup with a glass wool
plug and stainless-steel screen. This process involves sequential
extraction with the following recommended solvents in the listed
order.
     Water initial rinse: Place resin in a suitable
container, soak for approximately 5 min with Type II water, remove
fine floating resin particles and discard the water. Fill with Type
II water a second time, let stand overnight, remove fine floating
resin particles, and discard the water.
     Hot water: Extract with water for 8 hr.
     Methyl alcohol: Extract for 22 hr.
     Methylene chloride: Extract for 22 hr.
     Toluene: Extract for 22 hr.
     Methylene chloride: Extract for 22 hr.

    Note: You may store the resin in a sealed glass container filled
with toluene prior to the final toluene extraction. It may be
necessary to repeat the final methylene chloride extractions to meet
the cleanliness requirements in Section 13.1 of Method 23.
    2.2 You may use alternative extraction procedures to clean large
batches of resin. Any size extractor may be constructed; the choice
depends on the needs of the sampling programs. The resin is held in
a glass or stainless-steel cylinder between a pair of coarse and
fine screens. Spacers placed under the bottom screen allow for even
distribution of clean solvent. Clean solvent is circulated through
the resin for extraction. A flow rate is maintained upward through
the resin to allow maximum solvent contact and prevent channeling.
    2.2.1 Experience has shown that 1 mL/g of resin extracted is the
minimum necessary to extract and clean the resin. The aqueous rinse
is critical to the subsequent organic rinses and may be accomplished
by simply flushing the canister with about 1 liter of distilled
water for every 25 g of resin. A small pump may be useful for
pumping the water through the canister. You should perform the water
extraction at the rate of about 20 to 40 mL/min.
    2.2.2 All materials of construction are glass, PTFE, or
stainless steel. Pumps, if used, should not contain extractable
materials.

3.0 Drying

    3.1 Dry the adsorbent of extraction solvent before use. This
section provides a recommended procedure to dry adsorbent that is
wet with solvent. However, you may use other procedures if the
cleanliness requirements in Section 13.1 of Method 23 are met.
    3.2 Drying Column. A simple column with suitable retainers will
hold all the XAD-2 from the extractor or the Soxhlet extractor, as
shown in Figure B-1, with sufficient space for drying the bed while
generating a minimum backpressure in the column.
    3.3 Drying Procedure: Dry the adsorbent using clean inert gas.
Liquid nitrogen from a standard commercial liquid nitrogen cylinder
has proven to be a reliable source of large volumes of gas free from
organic contaminants. You may use high-purity tank nitrogen to dry
the resin. However, you should pass the high-purity nitrogen through
a bed of activated charcoal approximately 150 mL in volume prior to
entering the drying apparatus.
    3.3.1 Connect the gas vent of a liquid nitrogen cylinder or the
exit of the activated carbon scrubber to the column by a length of
precleaned copper tubing (e.g., 0.95 cm ID) coiled to pass through a
heat source. A convenient heat source is a water bath heated from a
steam line. The final nitrogen temperature should only be warm to
the touch and not over 40 [deg]C.
    3.3.2 Allow the methylene chloride to drain from the resin prior
to placing the resin in the drying apparatus.

    3.3.3 Flow nitrogen through the drying apparatus at a rate that
does not fluidize or agitate the resin. Continue the nitrogen flow
until the residual solvent is removed.
    Note: Experience has shown that about 500 g of resin may be
dried overnight by consuming a full 160-L cylinder of liquid
nitrogen.
[GRAPHIC] [TIFF OMITTED] TR20MR23.023

Figure B-1. XAD-2 fluidized-bed drying apparatus

PART 63--NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS
FOR SOURCE CATEGORIES

0
6. The authority citation for part 63 continues to read as follows:

    Authority:  42 U.S.C. 7401 et seq.

Subpart LL--National Emission Standards for Hazardous Air
Pollutants for Primary Aluminum Reduction Plants

0
7. In Sec.  63.849, revise paragraphs (a)(13) and (14) to read as
follows:

Sec.  63.849  Test methods and procedures.

* * * * *
    (a) * * *
    (13) Method 23 of Appendix A-7 of 40 CFR part 60 for the
measurement of Polychlorinated Biphenyls (PCBs) where stack or duct
emissions are sampled; and
    (14) Method 23 of Appendix A-7 of 40 CFR part 60 and Method 14 or
Method 14A in Appendix A to Part 60 of this chapter or an approved
alternative method for the concentration of PCB where emissions are
sampled from roof monitors not employing wet roof scrubbers.
* * * * *

Subpart EEE--National Emission Standards for Hazardous Air
Pollutants from Hazardous Waste Combustors

0
8. In Sec.  63.1208, revise paragraph (b)(1) to read as follows:

Sec.  63.1208  What are the test methods?

* * * * *
    (b) * * *
    (1) Dioxins and furans. (i) To determine compliance with the
emission standard for dioxins and furans, you must use:
    (A) Method 0023A, Sampling Method for Polychlorinated Dibenzo-p-
Dioxins and Polychlorinated Dibenzofurans emissions from Stationary
Sources, EPA Publication SW-846 (incorporated by reference--see Sec.
63.14); or
    (B) Method 23, provided in Appendix A, Part 60 of this chapter.
    (ii) You must sample for a minimum of three hours, and you must
collect a minimum sample volume of 2.5 dscm.
    (iii) You may assume that nondetects are present at zero
concentration.
* * * * *

Subpart XXX--National Emission Standards for Hazardous Air
Pollutants for Ferroalloys Production: Ferromanganese and
Silicomanganese

0
9. In Sec.  63.1625, revise paragraph (b)(10) to read as follows:

Sec.  63.1625  What are the performance test and compliance
requirements for new, reconstructed, and existing facilities?

* * * * *
    (b) * * *
    (10) Method 23 of Appendix A-7 of 40 CFR part 60 to determine PAH.
* * * * *

Subpart AAAAAAA--National Emission Standards for Hazardous Air
Pollutants for Area Sources: Asphalt Processing and Asphalt Roofing
Manufacturing

0
10. In table 3 to Subpart AAAAAAA of Part 63 revise the entry ``6.
Measuring the PAH emissions'' to read as follows:

           Table 3 to Subpart AAAAAAA of Part 63--Test Methods
------------------------------------------------------------------------
                 For * * *                       You must use * * *
------------------------------------------------------------------------

                                * * * * *
6. Measuring the PAH emissions............  EPA test method 23.
------------------------------------------------------------------------

* * * * *

PART 266--STANDARDS FOR THE MANAGEMENT OF SPECIFIC HAZARDOUS WASTES
AND SPECIFIC TYPES OF HAZARDOUS WASTE MANAGEMENT FACILITIES

0
11. The authority citation for part 266 continues to read as follows:

    Authority: 42 U.S.C. 1006, 2002(a), 3001-3009, 3014, 3017, 6905,
6906, 6912, 6921, 6922, 6924-6927, 6934, and 6937.

Subpart H--Hazardous Waste Burned in Boilers and Industrial
Furnaces

0
12. In Sec.  266.104, revise paragraph (e)(1) to read as follows:

Sec.  266.104  Standards to control organic emissions.

* * * * *
    (e) * * *
    (1) During the trial burn (for new facilities or an interim status
facility applying for a permit) or compliance test (for interim status
facilities), determine emission rates of the tetra-octa congeners of
chlorinated dibenzo-p-dioxins and dibenzofurans (CDDs/CDFs) using
Method 0023A, Sampling Method for Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans Emissions from Stationary Sources, EPA
Publication SW-846, as incorporated by reference in Sec.  260.11 of
this chapter or Method 23, provided in Appendix A-7, Part 60 of this
chapter.
* * * * *
[FR Doc. 2023-04958 Filed 3-17-23; 8:45 am]
BILLING CODE 6560-50-P


Comment Info: =================

General Comment: Dear Mr. Zeller:

I am writing as an individual consumer to request an extension of the comment period for the Food and Drug Administration's ("FDA") Proposed Rule Deeming Tobacco Products to be Subject to the Federal Food, Drug, and Cosmetic Act, as amended by the Family Smoking and Prevention and Tobacco Control Act (the "Proposed Rule") published at 79 Fed. Reg. 23,142 and Federal Register No. 2014-09491. On behalf of myself, I am requesting that the comment period for the Proposed Rule be extended by the FDA for an additional 105 days, from its current 75-day period, to 180 days.

The Proposed Rule raises a number of significant issues and questions that are important and relevant to me, as a consumer of products that are proposed for regulation under the Proposed Rule. The Proposed Rule asks about a hundred different questions I might want to respond to. I want to provide my thoughts and comments on many of these issues, but my time to devote to researching and providing thoughtful comments on these important questions is limited. I have already spent many hours researching and dissecting these issues, but they take time. I know that the FDA took many years to even come up with the Proposed Rule, so I do not think it is at all unreasonable to allow the public a mere six months to comment on it. This is our only opportunity, as consumers, to provide our feedback.

My doctor recommended to me that I try e-cigarettes.  I started in August 2013 and within a week, I went from a pack a day to one-half pack a day. I did my own research on e-cigarettes and found the studies from Australia and England that showed that e-cigarettes are safer than traditional cigarettes.

I realize that the FDA has the authority under 21 CFR 10.40 to extend this time frame and that the FDA has exercised this authority on numerous occasions in the past. I would therefore ask that you do so here, so that all stakeholders have the opportunity to provide their comments on this proposed regulation.

I appreciate your consideration of my request and am happy to discuss this issue with you further.