III. METHODS OF ANALYSIS
3.4. Quality Controls
57 Table 3.4. Limit of detection (LoD) for the PAHs
No. PAHs Conc. of
LoD (ng/μl)
Absolute amount
(pg)
1 Naphthalene 0,01 266
2 Acenaphthylene 0,08 1569
3 Acenaphthene 0,02 441
4 Fluorene 0,01 154
5 Phenanthrene 0,01 115
6 Anthracene 0,001 16
7 Fluoranthene 0,02 453
8 Pyrene 0,002 45
9 Benzo(a)anthracene 0,001 25
10 Chrysene 0,001 16
11 Benzo(b)fluoranthene 0,01 120
12 Benzo(k)fluoranthene 0,001 20
13 Benzo(a)pyrene 0,001 14
14 Dibenzo(a,h)anthracene 0,003 63
15 Benzo(g,h,i)perylene 0,004 79
16 Indeno(1,2,3-c,d)pyrene 0,002 35
58 Procedural efficiency was also checked with 16-PAH standard spiked method. 16 PAHs were spiked into the thimble blank for sediment and SPM, and Milli-Q water for dissolved PAHs. These spiked standards then proceeded through the step of procedural analysis. For the dissolved PAHs, the standard was spiked into 1000 ml of Milli-Q water plus 1% Methanol (solubility enhancement). The spiked waters were then aspirated through the SPE cartridges, and performed the step of analysis. The results were shown in the table 3.6 and 3.7. The recovery of spiked standards ranged from 63% (BaP) to 105% (ANTH) for the thimbles, and from 49% (BaP) to 96% (PHEN) for the water.
Table 3.6. Recovery of spiked PAH standards (16 PAH Mix 61) into the blank thimbles for sediment and SPM analysis. The data was calculated from the peak area of the ultraviolet detector response.
Compounds Spiked Mass Recovery Test (%)
(ng) 1 2 3 Mean
Naphthalene 500 111 89 101 100
Acenaphthylene 1000 101 109 99 103
Acenaphthene 500 108 96 83 96
Fluorene 100 98 94 89 94
Phenanthrene 50 93 98 89 93
Anthracene 50 96 119 101 105
Fluoranthene 100 87 98 94 93
Pyrene 50 76 138 95 103
Benzo(a)anthracene 50 85 107 82 91
Chrysene 50 93 101 85 93
Benzo(b)fluoranthene 100 93 95 93 94
Benzo(k)fluoranthene 50 114 91 91 99
Benzo(a)pyrene 50 35 49 104 63
Dibenzo(a,h)anthracene 100 93 90 100 94
Benzo(g,h,i)perylene 100 94 83 119 98
Indeno(1,2,3-c,d)pyrene 50 96 94 123 104
Table 3.7. Recovery of spiked PAH standards into the blank Milli-Q water for dissolved PAH analysis. The data was calculated from the peak area of the ultraviolet detector response.
Compounds Spiked Mass Recovery Test (%)
(ng) 1 2 3 Mean
Naphthalene 30000 47 82 88 72
Acenaphthylene 60000 92 96 99 95
Acenaphthene 30000 84 91 95 90
Fluorene 6000 102 100 103 101
Phenanthrene 3000 98 93 97 96
Anthracene 3000 108 106 112 109
Fluoranthene 6000 97 86 95 93
Pyrene 3000 93 83 93 90
Benzo(a)anthracene 3000 101 68 75 81
Chrysene 3000 94 64 66 75
Benzo(b)fluoranthene 6000 102 63 66 77
Benzo(k)fluoranthene 3000 74 44 48 55
Benzo(a)pyrene 3000 58 42 46 49
Dibenzo(a,h)anthracene 6000 106 53 53 71
Benzo(g,h,i)perylene 6000 104 52 53 70
Indeno(1,2,3-c,d)pyrene 3000 100 56 59 72
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