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The de termination of organochlorine pe sticide sand polychlorinated biphenyls in waters and

complex matrices (2000)

Methods for the Examinat ion of Waters and Associated M aterials 

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Table A1 Performance data generated using GC/ECD

Compound Spiked blank water Spiked river water LOD

Mean St Rec Mean St Rec

Aldrin 0.091 0.003 91 0.088 0.007 88 0.005

Dieldrin 0.095 0.005 95 0.90 0.007 90 0.009

Endrin 0.096 0.004 96 0.099 0.002 99 0.019

o,p’-DDE 0.094 0.005 94 0.093 0.005 93 0.019

p,p’-DDE 0.091 0.005 91 0.089 0.007 89 0.019

o,p’-DDT 0.091 0.003 91 0.083 0.004 83 0.009

p,p’-DDT 0.087 0.012 87 0.084 0.01 84 0.032

α-Endosulphan 0.093 0.003 93 0.088 0.004 88 0.009

β-Endosulphan 0.094 0.004 94 0.097 0.003 97 0.019

α-HCH 0.010 0.001 95 0.009 0.001 92 0.005

β-HCH 0.045 0.003 89 0.045 0.006 90 0.009

γ -HCH (lindane) 0.044 0.002 87 0.044 0.003 89 0.009

Heptachlor 0.091 0.005 91 0.085 0.007 85 0.009

p,p’-TDE 0.088 0.009 88 0.088 0.008 88 0.019

 Tecnazene 0.085 0.013 85 0.093 0.014 93 0.037

 Trifluralin 0.093 0.011 93 0.085 0.016 85 0.050Chlorothalonil 0.108 0.018 108 0.108 0.016 108 0.036

Propyzamide 0.098 0.015 98 0.091 0.006 91 0.036

 Triademefon 0.087 0.017 87 0.085 0.017 85 0.024

All values expressed in µgl -1 unless otherwise stated and based on analyses of 11 batches carried out in duplicate.

LOD is calculated from 4.65 x Sw of the spiked blank water which consisted of de-ionised water.

Data provided by Essex & Suffolk Water.

Additionally, hexachlorobutadiene, δ-HCH, ε-HCH, THE, diflufenican, isodrin, HCB, methoxychlor, cis-chlordane and

trans-chlordane can be analysed using LLE with pentane as solvent, giving similar performance data (information

provided by Southern Science Ltd).

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Figure B1 Typical GC/ECD chromatogram of a standard mixture of PCB

(PCB concentrations are approximately 200 µgl-1)

   C  o   u   n  t  s

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   P   C   B   3   1

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   P   C   B   2   8

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   P   C   B   5   2

   4

   T   H   E   (   i  n   t  e  r  n  a   l  s   t  a  n   d  a  r

   d   )

   5

   P   C   B   1   0   1

   6

   P   C   B   1   4   9

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   P   C   B   1   1   8

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   P   C   B   1   5   3

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   P   C   B   1   0   5

   1   0   P   C   B   1   3   8

   1   1   P   C   B   1   8   0

   3   5

   4   0

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   T   i  m  e   (   i  n  m   i  n

  u   t  e  s   )

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Figure B3 Typical selected ion mass chromatog ram of a standard mixture of PCB

(PCB concentrations are approximately 200 µgl-1)

   T   i  m  e   (   i  n  m   i  n  u   t  e  s   )

   A  b   u   n   d  a   n  c  e  (   %  )

   1   8  :   0   0

   2   0  :   0   0

   2   2  :   0   0

   2   4  :   0   0

   2

   6  :   0   0

   2   8  :   0   0

   3   0  :   0   0

   3   2  :   0   0

   3   4  :   0   0

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   0   5   1   0   1   5   2   0   2   5   3   0   3   5   4   0   4   5   5   0   5   5   6   0   6   5   7   0   7   5   8   0   8   5   9   0   9   5   1   0   0

   1

   P   C   B   3   1

   2

   P   C   B   2   8

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   P   C   B   5   2

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   P   C   B   1   0   1

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   P   C   B   1   4   9

   6

   P   C   B   1   1   8

   7

   P   C   B   1   5   3

   8

   P   C   B   1   0   5

   9

   P   C   B   1   3   8

   1   0

   P   C   B   1   8   0

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Table D1 Recoveries of PCB standard solutions using GC/ECD

Spiked ultrapure water Spiked tap water

PCB Added St Rec RSD LOD St Rec RSD LOD

spike (%) (%) (%) (%)

PCB 28 0.002 0.0002(12) 101 11.7 0.001 0.0002(12) 90 13.6 0.001

0.005 0.0005(11) 106 9.5 0.0005(12) 96 9.9

0.020 0.0020(12) 94 10.1 0.0010(15) 100 4.8PCB 52 0.002 0.0004(14) 115 15.5 0.002 0.0003(12) 121 11.8 0.001

0.005 0.0007(12) 113 13.1 0.0004(15) 106 7.7

0.020 0.0026(14) 98 13.4 0.0017(12) 102 8.2

PCB 101 0.002 0.0002(12) 98 8.4 0.0008 0.0003(12) 100 12.9 0.001

0.005 0.0005(12) 100 3.6 0.0003(12) 100 5.5

0.020 0.0026(12) 89 14.6 0.0007(12) 100 3.5

PCB 118 0.002 0.0001(12) 95 4.7 0.0004 0.0002(12) 94 9.4 0.0008

0.005 0.0002(12) 98 3.8 0.0004(15) 94 9.2

0.020 0.0026(15) 90 14.4 0.0009(15) 100 4.5

PCB 138 0.002 0.0003(14) 98 16.2 0.002 0.0002(12) 87 10.2 0.0008

0.005 0.0005(12) 101 10.9 0.0004(12) 90 4.7

0.020 0.0025(12) 85 14.6 0.0010(12) 99 5.3

PCB 153 0.002 0.0001(12) 100 5.5 0.0005 0.0002(14) 96 10.0 0.0009

0.005 0.0002(15) 99 4.1 0.0004(12) 90 8.1

0.020 0.0026(14) 88 14.9 0.0011(12) 97 5.9

PCB 180 0.002 0.0002(12) 94 8.1 0.0007 0.0002(12) 98 8.9 0.0008

0.005 0.0002(14) 101 4.9 0.0003(13) 93 6.9

0.020 0.0028(15) 82 17.1 0.0012(12) 100 5.9

All units expressed as µgl-1 unless otherwise specified.

LOD is calculated using 4.65 x Sw of the low spike.

Figure in brackets represents DF.

Data provided by Wessex Water.

Table D2 Number of possible isomers and per cent chlorine for the ten PCB groups

PCB group Empirical Molecular Number of Per cent

Formula weight possible chlorine

isomers by weight

monochlorobiphenyl C12H9Cl 188.5 3 18.8

dichlorobiphenyl C12H8Cl2 223 12 31.8

trichlorobiphenyl C12H7Cl3 257.5 24 41.3

tetrachlorobiphenyl C12H6Cl4 292 42 48.6pentachlorobiphenyl C12H5Cl5 326.5 46 54.3

hexachlorobiphenyl C12H4Cl6 361 42 58.9

heptachlorobiphenyl C12H3Cl7 395.5 24 62.8

octachlorobiphenyl C12H2Cl8 430 12 66.0

nonachlorobiphenyl C12HCl9 464.5 3 68.7

decachlorobiphenyl C12Cl10 499 1 71.2

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5000060000

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10 11 12 13 14 15 16 17 18 19 20

Time (in minutes)

45 

Figure E3 Mass chromatogram of ion 256 from figure E2 (GC-MS (SIM) of Cl3-PCB present in Aroclor 1242)

Figure E4 Mass chromatogram of ion 258 from figure E2 GC-MS (SIM) of Cl3-PCB present in Aroclor 1242)

Figure E5 Mass chromatogram of ion 291.9 from figure E2 (GC-MS (SIM) of Cl4-PCB present in Aroclor 1242)

   A   b  u  n   d  a  n  c  e

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Figure E6 Mass chromatogram of ion 289.8 from figure E2 (GC-MS (SIM) of Cl4-PCB present in Aroclor 1242)

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Figure G1 Typical large-volume injection GC/ECD chromatog ram of a standard PCB-organochlorine

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pesticide m ixture

  t  e  c  n  a  z  e  n  e

  h  e  x  a  c  h l  o  r  o  b  e  n  z  e  n  e

  P   C  B  2  8

  P   C  B  5  2

 i  s  o  d  r i  n

  P   C  B  1  0  1

  P   C  B  1  1  8

  P   C  B  1  5  3

  P   C  B  1  3  8

  P   C  B  1  8  0

   R  e  s  p  o   n  s  e  (    m  i  l  l  i   v  o  l  t  s  )

   T   i  m  e   (   i  n  m   i  n  u   t  e  s   )

   1   5

   7 .   5

   1   0 .   0

   1   2 .   5

   1   5 .   0

   2   0

   2   5

   3   0

   3   5

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