AVS AVS. FeS. Waters AVS. Ag 2 S

Transcript

1 BUNSEKI KAGAKU Vol. 59, No., pp The Japan Society for Analytical Chemistry 55 / H S HS S 4 5 Sep-pak C8 s 6 Acid Volatile Sulfide : AVS AVS Ag S Sep-Pak QMA s AVS 4 AVS : : : AVS 5 7 AVS AVS AVS FeS AVS 4 AVS

2 56 B U N S E K I K A G A K U Vol Sandy mud sample Glass syringe (0mL) Glass piston Plastic spoon Plastic syringe (5mL) (a) (b) (c) (d) Three way stopcock Slurry sample X Filter X De-oxygen Rubber cap Filtrate Glass bead 4 (e) (f) (g) Fig. Analytical procedure for determination of dissolved sulfide (H S, HS, S ) in sandy mud sediments : 5 ml plastic syringe ; : 0 ml glass syringe ; : 50 ml glass syringe ; : 0 ml glass syringe H S HS S H S 000 mgs L : 9 Na S 9H O.0 g 00 ml : ; N,N -p- N,N-dimethylp-phenylene diamine sulfate 0.4 g III 6 FeCl 6H O 0.6 g 6 M 00 ml ; N,N -p- 4.0 g g 6 M 00 ml 0.M : (CH COO) Zn H O.5 g CH COONa.5 g 50 ml Shimadzu UV-800 CF7D HA-80M H S HS : 5 ml, OD :.6 mm Fig. -a 0 ml, ID :.5 mm Fig. -b Fig. -c Fig. -d 0 ml Fig. -e Fig. -f DISMIC5- CS 0.45 μm Fig. -g 0 ml 0. M ml ZnS 6 M ml 0.5 ml nm ADVANTEC No. 5C 0 4 H S ml g 00

3 : / 57 Table Effect of the volume of de-oxygen (N ) added on analytical result for dissolved sulfide (H S, HS ) in sandy mud sediments de-oxygen Dry weight Theoretical interstitial Dilution rate Concentration RSD (n ) RSD (n ) ml g ml mgs L The sample was taken from west of Lake Nakaumi on June, 008. H S HS : 0 ml 50 ml 0 ml Fig. -f H S 50 ml 50 ml 0 ml ml g ml ml ml ml ml ml RSD n Table 50 ml 0 ml ml Table RSD : RSD ml 0 ml A B A B RSD. 4.4 Table rpm 8 0 Table

4 58 B U N S E K I K A G A K U Vol Table Effect of the amount of sediment sample used on analytical result for dissolved sulfide (H S, HS ) in sandy mud sediments Sample de-oxygen Dry weight Theoretical interstitial Dilution rate Concentration ml g ml mgs L RSD A a) B b) a) The sediment sample A was taken from center of Lake Nakaumi on June 9, 008. b) The sediment sample B was taken from west of Lake Nakaumi on June, 008. Table depth Comparison of the centrifugation method and the proposed method Concentration by centrifugation cm mgs L by syringe The sediment sample was taken from west of Lake Nakaumi on June, ml 9.4. ml ml ml. 4.9 Table ml 4.0 μgs.0 μgs RSD n μgs.0 μgs Table 4 Separation rate using the centrifugal separation device depth () Before centrifugation Total weight Weight () After centrifugation Weight after decantation () Collected () () Theoretical interstitial volume Separation rate a) cm g g g (ml) ml a) Collected volume divided by theoretical interstitial volume

5 : / 59 Table 5 Recovery of dissolved sulfide added to mud sample ( : 68.0 ) Sample Found Recovery weight (wet) Average RSD (n 5) Average g μgs μgs μgs μgs Mud The sample was taken from center of Lake Nakaumi on June 9, 008. Table 6 Sample Recovery of dissolved sulfide added to sandy mud sample ( : 4.0 ) Found Recovery weight (wet) Average RSD (n 5) Average g μgs μgs μgs μgs Sandy mud The sandy mud sample was taken from west of Lake Nakaumi on June, RSD 5..5 Table 5 RSD Table Free-H S H S HS AVS 7 AVS Free-H S mgs L 0.8 mgs L Fig. 7 8 A : 9006 : :

6 60 B U N S E K I K A G A K U Vol depth / cm Free-H S / mgs L AVS / mgs g-dry - Fig. Vertical distributions of Free-H S (H S HS ) in the interstitial and AVS in the bottom sediment at the northeast of Ariake Bay : Free-H S (008/7/8); : AVS (008/7/8); ; Free-H S (008//); : AVS (008//) p. 7 (005). ) Raquel, Vaquer-Sunyer, C. M. Duarte : Limnol. Oceanogr., 55 (), 075 (00). ) J. D. Cline : Limnolo. and Oceanogr., 4, 454 (969). 4) JIS K 00 : (99). 5) : (Bunseki kagaku), 46, 9 (997). 6) M. Okumura, N. Yano, K. Fujinaga, Y. Seike, S. Matsuo : Anal. Sci., 5, 47 (999). 7) E. N. Leonard, V. R. Mattson, D. A. Benoit, R. A. Hoke, G. T. Ankley : Hydrobiologia, 7 (), 87, 99. 8) Tanmay Praharajand, Danielle Fortin :, Air, & Soil Pollution, 55, 5 (004). 9) Gerard A. van den Berg, J. P. Gustav Loch, Lambertus M. van der Heijdt, John J. G. Zwolsman : Environ. Toxicol. Chem., 7 (4), 758 (998). 0) Tao Fang, Xiangdong Lia, Gan Zhangc : Ecotoxicol. Environ. Saf., 6, 40 (005). ) M. Okumura, M. Yata, K. Fujinaga, Y. Seike : Japan Association of Ion Exchange, 4,, (00). ) W. Davison, J. P. Lishman : Analyst, 08, 5 (98). ) H. Maeda, A Kawai : Nippon Suisan Gakkaishi, 54 (9), 6 (988). 4) G. Kanaya, E. Kikuchi : Hydrobiologia, 58, 87 (004). 5) : (), 0 (008). 6) : (), 5 (008). 7) : 74 (), 40 (008). ) :

7 : / 6 A Simple in situ Extraction Method for Dissolved Sulfide in Sandy Mud s Followed by Spectrophotometric Determination and Its Application to the Bottom at the Northeast of Ariake Bay Shogo SUGAHARA, Tatsuya YURIMOTO, Kazuhiro AYUKAWA, Katsunori KIMOTO, Yukiko SENGA, Minoru OKUMURA and Yasushi SEIKE Faculty of Science and Engineering, Shimane University, 060, Nishikawatsu-cho, Matsue-shi, Shimane Seikai National Fisheries Research Institute, 55-8, Taira-machi, Nagasaki-shi, Nagasaki 85- Faculty of Geo-Environmental Science, Rissho University, 700, Magechi, Kumagaya-shi, Saitama (Received 4 July 00, Accepted 5 November 00) We developed a simple in situ extraction method for dissolved sulfide (H S, HS, S ) in sandy mud sediments. All analytical procedures were performed in a sealed system of glass syringes to prevent the volatilization of hydrogen sulfide and the oxidation of sulfide by air. An adequate amount of sandy mud sediment was put in a graduated glass syringe on site immediately after sampling. This procedure was performed using a unique and useful tool ; a plastic syringe had its front portion cut, so as to avoid the attachment of sediment to the inside wall of the syringe. To the sediment sample in the syringe, distilled, deoxygenated by babbling with nitrogen gas, was injected via a three-way stopcock with another syringe. After mixing well, the sample was filtrated into the other syringe through a filter (0.45 μm). In addition, zinc acetate solution was added to the filtrate in the syringe, and was then spectrophotometrically determined by the methyleneblue method after being brought back to laboratory. The proposed method was successfully applied to bottom sediment samples taken from northeast of Ariake Bay. A high concentration of dissolved sulfide was detected in a warmer season. This method should be useful to evaluate sediment quality and to assess the influence of dissolved sulfide on benthos such as bivalves. Keywords : in situ extraction method of dissolved sulfide ; sandy mud sediment ; methyleneblue method ; interstitial.