106
Marine Sediments
4.4.9
Basic Organic Compounds
Kido et al. [315] determined basic organic compounds such as quinoline, acridine,
aza-fluorene, and their N-oxides in marine sediments found in an industrial area. The
sediments were extracted with benzene by using a continuous extractor for 12 h.
Hydrochloric acid solution (1 N) was added to the benzene extracts, and the mixture
was shaken for 5 min; the acid layer separated from the benzene layer was made
alkaline by the addition of sodium hydroxide, and the alkaline aqueous solution was
extracted with diethyl ether; the ether extracts were then dehydrated with anhydrous
sodium sulphate and concentrated with a Kuderna-Danish evaporator. The concentrations were separated and analysed by gas chromatography-mass spectrometry and
gas chromatography high resolution mass spectrometry.
4.4.70
Organosulphur Compounds
Dichloroethane extraction of the sediment, followed by elimination of elemental
sulphur, mercaptans, disulphide and dibenzo-thiophene on a copper column is followed by a gas chromatographic analysis with flame photometric detection of the
organosulphur compounds. The detection limit is 1 ng as sulphur with a precision of
± 10 % [317]
Table 4.8
Standard reference sediment NBS SRM 1645 (from [316))
Compound
Naphthalene
Hexachlorobutadiene
Acenaphthylene
Acenaphthene
Fluorene
Diethyl phthalate
Hexachlorobenzene
Phenanthrene
Anthracene
Di-n-butyl phthalate
Fluoranthene
Pyrene
n-Butyl benzyl phthalate
Benz (a) anthracene plus chrysene
Bis (2-ethylhexyl) phthalate
Benzo (a) pyrene
p, p-DDE
p,p-DDD
p, p-DDT
PCB as Aroelor 1254
Benzo (k, h) fluoranthene
Mean concentration, mg/kg dry,
X (%RSD)
n=3
0.254 (16)
ND
0.092 (14)
0.173 (6)
1.93 (4)
ND
ND
3.06 (3)
0.80 (9)
0.66 (14)
27.5 (5)
58.7 (5)
0.51 (13)
104 (6)
0.58 (15)
75 (7)
0.447 (7)
0.83 (11)
3.24 (2)
1.23 (34)
31.6 (8)
Recovery %
15 ± 6
69 ± 5
56 ± 5
71± 4
77± 2
69 ± 5
59 ± 8
84 ± 5
67 ± 4
179 ± 3
77±
83 ±
78 ± 4
77 ± 10
Marine Sediments
4.4.9
Basic Organic Compounds
Kido et al. [315] determined basic organic compounds such as quinoline, acridine,
aza-fluorene, and their N-oxides in marine sediments found in an industrial area. The
sediments were extracted with benzene by using a continuous extractor for 12 h.
Hydrochloric acid solution (1 N) was added to the benzene extracts, and the mixture
was shaken for 5 min; the acid layer separated from the benzene layer was made
alkaline by the addition of sodium hydroxide, and the alkaline aqueous solution was
extracted with diethyl ether; the ether extracts were then dehydrated with anhydrous
sodium sulphate and concentrated with a Kuderna-Danish evaporator. The concentrations were separated and analysed by gas chromatography-mass spectrometry and
gas chromatography high resolution mass spectrometry.
4.4.70
Organosulphur Compounds
Dichloroethane extraction of the sediment, followed by elimination of elemental
sulphur, mercaptans, disulphide and dibenzo-thiophene on a copper column is followed by a gas chromatographic analysis with flame photometric detection of the
organosulphur compounds. The detection limit is 1 ng as sulphur with a precision of
± 10 % [317]
Table 4.8
Standard reference sediment NBS SRM 1645 (from [316))
Compound
Naphthalene
Hexachlorobutadiene
Acenaphthylene
Acenaphthene
Fluorene
Diethyl phthalate
Hexachlorobenzene
Phenanthrene
Anthracene
Di-n-butyl phthalate
Fluoranthene
Pyrene
n-Butyl benzyl phthalate
Benz (a) anthracene plus chrysene
Bis (2-ethylhexyl) phthalate
Benzo (a) pyrene
p, p-DDE
p,p-DDD
p, p-DDT
PCB as Aroelor 1254
Benzo (k, h) fluoranthene
Mean concentration, mg/kg dry,
X (%RSD)
n=3
0.254 (16)
ND
0.092 (14)
0.173 (6)
1.93 (4)
ND
ND
3.06 (3)
0.80 (9)
0.66 (14)
27.5 (5)
58.7 (5)
0.51 (13)
104 (6)
0.58 (15)
75 (7)
0.447 (7)
0.83 (11)
3.24 (2)
1.23 (34)
31.6 (8)
Recovery %
15 ± 6
69 ± 5
56 ± 5
71± 4
77± 2
69 ± 5
59 ± 8
84 ± 5
67 ± 4
179 ± 3
77±
83 ±
78 ± 4
77 ± 10