Organic compounds in non-saline sediments 159
6.8 MISCELLANEOUS ORGANIC COMPOUNDS
6.8.1 Humic and fulvic acid
Klenke et al [197] described a technique for extraction of humic and fulvic acids from
stream sediments and outlined methods for their determination.
Hayase et al [198] applied reverse phase liquid chromatography to the examination
of molecular weight fractioned sedimentary fulvic acid.
6.8.2 Detergents
Ambe and Hanya et al [51] have combined the Longwell and Maniece et al [52] methods using methylene blue with the infrared spectroscopic method of Sallee et al [53] to
devise a method for the determination of alkylbenzene sulphonates. Methylene blue
alkylbenzene sulphonate complexes give absorption peaks at 980 and 1010 cm
−1 , the
ratio of the heights being proportional to the ratio of the amount of sulphonate to the
total amount of methylene blue sensitive substances in the complex. The filtered sample is shaken (50 ml) with 0.1 N sulphuric acid (1 ml), 0.025% methylene blue solution
(1 ml) and 1,2-dichloroethane (20 ml) for 1 minute. After washing the separated
organic layer twice with 20 ml of 0.0013% solution of methylene blue in 0.004 N
sulphuric acid also containing 0.022% of silver sulphate, its extinction is measured
at 655 nm to give the total amount of substances active towards methylene blue. The
organic layer is evaporated to dryness prior to pelleting with potassium bromide and
examination by infrared spectroscopy.
This method has been applied to bottom sediments and muds [54]. The mud
sample is centrifuged to separate the water, dried at room temperature, ground, and
sieved. This residue is extracted for 1 hour at 80
◦ C with methanol-benzene (1:1),
the extraction is repeated twice and the combined extracts are evaporated and the
residue dissolved in water. Alkylbenzenesulphates are then determined by infrared
spectroscopy as described above.
6.8.3 Optical whiteners
The three most important detergent fluorescent whitening agents are solid under the
trade name DAS 1, DBP and BLS (diaminostilbene, distryrybiphenyl and bleach stable.
The composition of these compounds is DAS 1,4,4’-bis [4-anilino-6-morpholino1,3,5-triazin-2-yl)-amino] stilbene-2,2’-disulphonate; DSBP, 4,4’-bis (2-sulfostyryl);
BLS, 4,4’-bis (4-chloro-3sulfostyryl)biphenyl.
Uchiyama et al [62] has given details of a spectrofluorimetric procedure for the
isolation and determination of down to 0.2 mg kg
−1 of fluorescent whitening agents
in extracts of bottom deposits. The fluorescent whitening agents were sodium salts of
a sulphonated stilbene derivative and this was measured by fluorescence (excitation
370 nm, emission 405 nm) with the use of tetra-n-butyl ammonium hydroxide.
Uchiyama et al [62] applied this method to the determination of fluorescent
whitening agents and alkyl benzenesulphonates and also methylene blue active substances in bottom sediment samples taken in a lake. The muds were filtered off with
a suction filter and frozen until analysed. The wet bottom mud was extracted three
6.8 MISCELLANEOUS ORGANIC COMPOUNDS
6.8.1 Humic and fulvic acid
Klenke et al [197] described a technique for extraction of humic and fulvic acids from
stream sediments and outlined methods for their determination.
Hayase et al [198] applied reverse phase liquid chromatography to the examination
of molecular weight fractioned sedimentary fulvic acid.
6.8.2 Detergents
Ambe and Hanya et al [51] have combined the Longwell and Maniece et al [52] methods using methylene blue with the infrared spectroscopic method of Sallee et al [53] to
devise a method for the determination of alkylbenzene sulphonates. Methylene blue
alkylbenzene sulphonate complexes give absorption peaks at 980 and 1010 cm
−1 , the
ratio of the heights being proportional to the ratio of the amount of sulphonate to the
total amount of methylene blue sensitive substances in the complex. The filtered sample is shaken (50 ml) with 0.1 N sulphuric acid (1 ml), 0.025% methylene blue solution
(1 ml) and 1,2-dichloroethane (20 ml) for 1 minute. After washing the separated
organic layer twice with 20 ml of 0.0013% solution of methylene blue in 0.004 N
sulphuric acid also containing 0.022% of silver sulphate, its extinction is measured
at 655 nm to give the total amount of substances active towards methylene blue. The
organic layer is evaporated to dryness prior to pelleting with potassium bromide and
examination by infrared spectroscopy.
This method has been applied to bottom sediments and muds [54]. The mud
sample is centrifuged to separate the water, dried at room temperature, ground, and
sieved. This residue is extracted for 1 hour at 80
◦ C with methanol-benzene (1:1),
the extraction is repeated twice and the combined extracts are evaporated and the
residue dissolved in water. Alkylbenzenesulphates are then determined by infrared
spectroscopy as described above.
6.8.3 Optical whiteners
The three most important detergent fluorescent whitening agents are solid under the
trade name DAS 1, DBP and BLS (diaminostilbene, distryrybiphenyl and bleach stable.
The composition of these compounds is DAS 1,4,4’-bis [4-anilino-6-morpholino1,3,5-triazin-2-yl)-amino] stilbene-2,2’-disulphonate; DSBP, 4,4’-bis (2-sulfostyryl);
BLS, 4,4’-bis (4-chloro-3sulfostyryl)biphenyl.
Uchiyama et al [62] has given details of a spectrofluorimetric procedure for the
isolation and determination of down to 0.2 mg kg
−1 of fluorescent whitening agents
in extracts of bottom deposits. The fluorescent whitening agents were sodium salts of
a sulphonated stilbene derivative and this was measured by fluorescence (excitation
370 nm, emission 405 nm) with the use of tetra-n-butyl ammonium hydroxide.
Uchiyama et al [62] applied this method to the determination of fluorescent
whitening agents and alkyl benzenesulphonates and also methylene blue active substances in bottom sediment samples taken in a lake. The muds were filtered off with
a suction filter and frozen until analysed. The wet bottom mud was extracted three