Trace Metal Levels in Intertidal Molluscs of California Abstract Determinations of Ag, Cd, Cr, Cu, Mn, Pb, and Zn were made by atomic absorption spectrophotometry on 7 species of Mollusca in the genera Acmaea, Tegula, Thais (gastropods), and Mytilus, Protothaca, and Tapes (bivalves). Eleven regions along the California coast from San Francisco Bay to Los Angeles were included. Separate analyses were performed on shells, and on soft portions of whole bodies. Highest levels, above 900 ppm Pb were found in bodies of Acmaea digitalis, 570 ppm Cu and 1700 ppm Zn in bodies of Thais emarginata. Trace Metal Levels in Intertidal Molluscs of California Introduction A growing number of observations of potentially toxic levels of trace elements such as lead, cadmium, and zinc in fishes and shell¬ fish has focused concern on the matter of distribution of these materials in marine organisms (Drinnan, 1966; Hardy, 1966; Houblouget al, 1954; MeFarren et al, 1961). The interest in this field is not new. Since the work of Cornec (1919), and Clark and Wheeler (1922), scientists have been aware of concentration of trace metals in a variety of marine plants and animals. Results of later studies have been compiled by Vinogradov (1953) and Goldberg (1965); they cover many marine species, though most of the data were obtained by analytical methods far less accurate than those in current use. Limited information is now available on the heavy metal content of a number of marine molluscs in various parts of the world (e.g. Brooks and Rumsby, 1965; Shuster and Pringle, 1968) but little has been done with California species. In the present study, 7 species of molluscs from 11 locations in California were analyzed for their content of silver, cad- mium, chromium, copper, manganese, lead, and zinc (Ag, Cd, Cr, Cug Mn, Pb, Zn). While far from Comprehensive, the present survey represents an attempt to establish baselines for existing levels, to relate these levels to possible environmental sources, and to discover any molluscs which exhibit particularly high levels of one or more metals. Materials and Methods Collecting stations are shown in Fig. 1. The species examined -2- included two herbivorous gastropods, one predatory snail, two bivalves living on hard substrata, and two burrowing clams, as follows: Acmaea digitalis Eschscholtz, 1833 Tegula funebralis (Adams, 1854) Thais emarginata (Deshayes, 1839) Mytilus californianus (Conrad, 1837 tilus edulis Linnaeus, 1758 Protothaca staminea (Conrad, 1837) Tapes semidecussata (Reeve, 1864) All species were collected alive, from the lowest portions of their intertidal ranges. Animals were kept in filtered sea water for 24 hours to purge sediments and gut contents. Before removal of soft parts, com¬ mensal organisms were removed, and the external surfaces of the shells were cleaned with a non-metallic brush. Bivalves were placed in a 60°0. oven for 15 minutes to cause opening, while gastropods were cracked carefully in a vice. Bodies of both classes were then excised withaa plastic knife, and both bodies and shells were washed with filtered sea water and dried at 110°0. for 24 hours. The bodies of each species from each location were pooled together to produce enough material for anal¬ ysis. From this, 3 aliquots were taken for triplicate analysis. The same was done for shells. Each aliquot of shell was crushed with mortar and pestle to.5-1cm pieces. Samples of approximately .25g were used for analysis, as experience showed that this small amount of sample, in the dilutions used, caused less light scattering in analysis. These samples were then placed in a 30ml pyrex beaker and weighed to the nearest .lmg. Five 196 to oml of concentrated HOlwere added and the beaker covered with a way watch glass. After foaming subsided, 5-6ml of 90% HNO3 were added. Samples were shaken gently and warmed at low heat (60-70°0.) When solutions turned clear, they were diluted with distilled water to 25ml. Dried bodies were ground to a fine powder. Aliquots of approx- imately lg were weighed to the nearest .lmg in a 30ml pyrex beaker. Then 5-6ml of 70% HNO, were added; samples were covered as above, and heated to a slow boil. If lipids were not present (visible as droplets) samples were allowed to cool, and 2-3ml of 30% H,0, were added dropwise to oxidize remaining organic matter. When clear, solutions were diluted with distilled water to 25ml. If lipids were present, samples were evaporated to dryness, then charred at 250°0. They were then cooled to room temperature, redissolved in 90% HNO, boiled, recooled, treated as above with Ho0, then diluted to 25ml. Controls were run in two different ways, all steps of treatment being identical to those with samples. Type 1 controls were blank beakers used to compensate for contamination of samples from procedures (handling, drying, reagents, etc.). These readings were subtracted from sample readings. Type 2 controls were beakers containing standard solutions of mètals at known concentrations, to measure loss. Steps of treatment were again identical to those with samples. Results, used to adjust sample readings, are as follows: Ag-1% loss, Cd-no loss, Or- 7 gain, Cu-7% loss, Mn-5% loss, Pby11% loss, Zn-38 loss. Gderk All samples were analyzed using a Perkin-Elmer Atomic Absorption Spectro- photometer, Model 303. Light scattering artifacts in Od, Pb, and Zn were compensated for by running all samples with the Pb lamp at 222). At this wavelength, the spectrophotometer read only background levels of light scatter. Values from this procedure were treated as werettypell controls, and subtracted from sample readings. -H Results and Discussion Levels of metals found in shells and bodies appear in tables 1 and 2, and figs. 2 and 3, and are discussed below. Silver and Copper Of the metals studied, Ag was distributed most uniformly in the shells of animals examined; the highest levels,210 ppm, were found in Acmaea at Fort Point, San Francisco (location B, in figs. and tables); Thais and Tegula at Mussel Point (G). Body values of Ag were highest in Tapes from Coyote Point, San Mateo (A), 7.3 ppm. Detectable amounts (21 ppm) were found in all Tegula bodies, and consistently higher values in the shells. Nicholls et al. (1959) have found Ag in zooplankton; Brooks and Rumsby (1965) suggest that Ag is introduced into the digestive system of the animals they studied (bivalves Ostrea sinuata, Pecten novae-zelandiae and Mytilus edulis) by ingestion of plankton and suspended particles. Copper levels on molluscan bodies examined were up to 90 times as high as in the shells (viz. Thais). High Cu values in Tegula,175 ppm, and Thais, 570 ppm, from Fisherman's Wharf at Monterey Harbor (F) are probably related, at least in part, to the presence of nearly 300 small boats docked in the area, some only 50 yards away; the hulls of many are coated with a Cu-based anti-fouling paint. The almost three-fold increase in hais over Tegula may be related to the fact that the former is a preda- cious snail and may get part of its Cu from the ingestion of herbivores (like Tegula) or filter feeders (like Mytilus) which already contain sig- nificant levels of Cu. Copper is an important enzyme activator and is a constituent of hemocyanins that are present in all of the molluscs studied. A basic physiological level for Cu cannot now be suggested, owing to the 198 -5 likely possibility of Cu contamination at all localities in this study. Chromium and Manganese Chromium was found in relatively high amounts in bodies at two local- ities, in Acmaea at Fort Point (B) and in Tegula at Fisherman's Wharf (F). Shells were consistently highest at the Wharf. Body levels may relate to possible contamination from automobiles at Fort Point (see lead, below), and the presence of small craft in Monterey Harbor (see copper, above). Tapes at Coyote Point (A) is also notable. tor high Cr. High Mn levels in bodies and shells were found in animals from muddy areas; in Mytilus and Tapes at Coyote Point (A) and in Mytilus at Elkhorn Slough (D). Values were also high in Acmaea from Fort Point (B) and White's Point (K). Manganese levels in shells of Tegula were first documented by Krinsely (1959) who found 4-6 ppm in shells of live California animals, and 13-17 ppm in fossilized specimens. Most values in the present study are above the range given for live animals. Manganese has a role as an activator of enzyme systems that is well established. Lead Detection of Pb in shells was partially handicapped by high spectro- photometric limits. High values were found in Mytilus californianus at Half Moon Bay (C), both species of Mytilus at White's Point (K), and especially in Acmaea at Fort Point (B), 931 ppm. These are animals which live well up in the intertidal zone, and, near cities, they are exposed to atmospheric fallout of Pb from automobile exhaust for much of the day. Animals found at Half Moon Bay were in the vacinity of a sewer outfall. White's Point, besides being directly inshore of the Los Angeles County sewer outfall, is close to regions of heavy traffic in Los Angeles and Long Beach. Fort Point attracts an estimated 60-100 tourist automobiles 199 -6- per day on weekends, many of which have been seen to park within 5 feet of the wall on which Acmaea were found. In addition, this locality is situated directly under the Golden Gate Bridge. The very high levels of Pb in Acmaea digitalis bodies at this point perhaps reflect not only the high Pb fallout from auto exhaust, but also the fact that this species lives on, and feeds from rock surfaces not thoroughly rinsed by their submersion at high tides each day. Lead has no known usefulness in bio- logical systems, and is known to inhibit certain enzymes. Cadmium and Zinc Cadmium in shells was highest in Mytilus at Carmel Bay (I), in Tapes at Coyote Point (A), and Tegula at Fisherman's Wharf (F). Body values are most sizable in Acmaea at White's Point (K) and Thais at the Wharf (F). Cadmium is toxic to living systems because it can replace Zn, an important component of metalloproteins such as carbonic anhydrase. Zinc metal in the environment, however, often contains substantial amounts of Od as a contam¬ inant, which might explain the high correlations of Cd and Zn in bodies of maea and Thais. Zinc was the most abundant trace metal in the soft parts of molluscs, as it is in seawater; values in the body were at least 20 times higher than in the shell. High amounts of Zn in bodies of Thais at Fisherman's Wharf, 1700 ppm, and of Acmaea at White's Point (K), 763 ppm, may be correlated with location. In motor-driven marine vessels, it is almost universal to have Zn blocks fastened to the hull, near the propeller to protect it and the drive shaft from electrolysis in sea water. These blocks, higher in the electromotive-force series than iron and brass, slowly go into solution and need replacement at regular intervals. Fisherman's Wharf, as noted earlier, lies in a harbor, while at White's Point (K) the collecting siteer. 200 -7- is less than 4 miles from the Los Angeles-Long Beach Harbor, where many hundreds of boats are moored. Zinc has been found to be concentrated by brown algae (Black and Mitchell, 1952) 40 times that in sea water. Mytilus edulis It is perhaps noteworthy that levels of trace metals in Mytilus edulis from California show a number of agreements with those of the same species in New Zealand (Table 3) as determined by Brooks and Rumsby (1965). Dif- ferenceslocalities and methods of analysis, however, should be taken into consideration in any comparisons made. Summary Determinations of Ag, Cd, Cr, Cu, Mn, Pb, and Zn were made by atomic absorption spectrophotometry on 7 species of Mollusca in the genera Acmaea, Tegula, Thais (gastropods), and Mytilus, Protothaca, and Tapes (bivalves). Eleven regions along the California coast from San Francisco Bay to Los Angeles were included. Separate analyses were performed on shells and soft portions of whole bodies. Highest levels. above 900 ppm Pb found in bodies of Acmaea digitalis, 570 ppm Cu in Tegula funebralis and 1700 ppm Zn in Thais emarginata, have raised the question of causes for these unusual levels. 20 -8 Figure Captions Figure 1. Map of collection sites, coast of California. A. Coyote Point, San Mateo, San Francisco Bay. Mud flats with some rocks; wave action slight. B. Fort Point, San Francisco. Animals collected from vertical concrete sea wall below Golden Gate Bridge; moderate wave action. Half Moon Bay. Animals collected from rocky area just north of Pillar Point, not far from sewer outfall for towns of Princeton, Miramar, and Half Moon Bay; moderate to strong wave action. Sandy mud flats; no wave action. Elkhorn Slough, Moss Landing. Monterey Municipal Wharf, Monterey. Animals collected from rocks immediately to right of wharf. Mixing with waters inside the harbor present; moderate wave action. Fisherman's Wharf, Monterey. Animals collected from rocks immediately to the right of, and underneath, wharf. This region, inside the small craft harbor, is in close proximity to some 300 boats; no wave action. Mussel Point, Pacific Grove, site of Hopkins Marine Station. Animals collected from intertidal rocks; moderate wave action, H. Point Pinos, Pacific Grove, Animals collected within 30 ft. ofnt mouth of Pacific Grove sewage treatment plant outfall; wave action moderate to strong. Carmel Bay. Animals collected from rocky-intertidal region, close to City of Carmel sewage treatment plant outfall; moderate to strong, wave action. Point Sur, Monterey County. Animals collected from rocky-intertidal; wave action moderate to strong. K. White's Point, Palos Verdes Peninsula, Los Angeles. Animals collected on intertidal rocks directly inshore of mile-long Los Angeles County sewer outfall; wave action moderate to strong. Figure 2. Concentrations of trace elements in shells of California molluscs (pom dry weight). Letters indicate collecting sites shown in Fig. 1. Dashed lines indicate detection limits. Figure 3. Concentrations of trace elements in bodies of California molluscs (ppm dry weight). LLetters indicate collecting sites shown in Fig. 1. Dashed lines indicate detection limits. 63 -9- Table Captions Table 1. Concentrations of trace elements in shells of California molluscs (ppm dry weight). N - no. of individuals in pooled sample. Values given for each sample are means and standard deviations for analysis of 3 separate aliquots. Letters indicate collecting sites shown in Fig. 1. Table 2. Concentrations of trace elements in bodies of California m molluscs (ppm dry weight). N - no. of individuals in pooled sample. Values given for each sample are means and standard deviations for analysis of 3 separate aliquots. Letters indicate collecting sites shown in Fig. 1. Table 3. Trace metals (ppm dry weight) in soft portions of whole bodies of Mytilus edulis. Values show means followed by ranges in parentheses. A. Levels found in present study. B. Levels found by Brooks and Rumsby (1965) in New Zealand, 203 Pacitic Ocean A-Coyote Point B-Fort Point C-Half Moon Bay D-Elkhorn Stough E-Monterey Wharf +2 F-Fisherman's Wharf (Mty.) G-Mussel Point A-Point Pinos -Carmel Outfall -Point Sur K-White’s Point Los Angeles San Pedro Channel „ L Monterey Bay 6 3 -0- 207 Fi9 S San Francisco Bay -11- —— r- RHO D R R 1r — MU o G oo A --.- NOOO O C OOROOo o o . + 1114 1+ 1+ ++++++ ++++++ 4 ONNN OHOO OE O se 7e 6 GO NO 1+ • | | + • ++- • + ++ ++ O C O o OO + + o . AA A AA GNGG OO O + EEN —. OVO J OE - ON.O.. O O G OO NO 4 111 1+1 + 1+ +* Oo OO O O O O . . . .. O. . + oO 0. C- DO O 1+ +1FI+H1+ ++ H- I+1+ +* ++ + —. OOP- ON OO P 0 O O 1 . RA 8 RARR * . 14 O oo O ooooO+ +OO OOH PON O NHO ON OODO O r. DON + D No — Table 1 5 8 5 29 5 80 C -12 50 —0- OO G oo o PONO . . OA O — * * * + . + . ++++ ++ ++ + ( oooo0 O N EENE — O NONNE . . • ROOON O ++ + + • ++ + ++ + . . OO N ONOOO O NO NN + . + + + + + + * . . . C O oo NO L oO. N Oo GOO. N OF ++ ++++1 A++ ++ + +H O . . . . . O Oooo O NR OON O . . O ). . O O O NE + + ++ + ++ +* Ec N NR. —0. O C AA NOA NN NNNN D N + +++ . . . H + + NNNNE N OO C NE NAONN UOON ON O O O o ++ + ++ 1 + + + OO + + ++ + OOOO Table 2 5 — 99 8 15 . O8 1 — 5 3 8 206 . 1 -13- 207 — S MAIAHATITLTE â â — r 10d — — M-PE-H- — 20 + Cr ++ — ------+-1-- — — — — LAHEA — — — — — H.- — — HHE 11 — — — — — 1— — InEIMEMAIIIIAILHA 1 — — Z S ——— ——— 11 1----- HE L FG hk i CK CAER 6 K 8 K AEKD Fig: 2 (c -1l- LEREHRH Cd LLATHRAIALE Cr MLL MRAEA-HEA Mn CHAEELIALILELILETLLLALELEIHELA Cu lnnialhnE H 10 300 00. 411- LAEILLLIAEL 111 Z 20 A. -15 Table 3 — — Cu Mn Ag Pb Ca 28 (201- Calif. 4 (2-8) 24 5 (3-7) 1.0(1-3) 7 (5-11) 16(6-28 5 (2-8) 31) New (50- 6 1(71-1.99 (8-11) 1669-24) 27(12-39 12(3-25) 10 ( 1091 180) 1Zealand 209 -16 The author wishes to express thanks to the faculty, staff, and graduate students of Hopkins Marine Station, especially to Dr. Donald P. Abbott for his encouragement and many indispensible suggestions both during research and while writing the manuscript. Dr. John H. Martin provided additional helpful criticism and a general knowledge of the problems of trace metal analysis. Both to them and to Mr. George Knauer and Mr. S. John Chang, I owe gratitude for inspiration furnished during this study. C -17- Literature Cited Black, William Aird Poden åp Robert Lyell Mitcholl Trace oloments in the common browm al 1952. ac and sea water. 5-58 Journ. Marine Biol. Assoc. U. K. 30: Brooks, Robort R. & Martin Cregory Rumsby 1965. The biogeochomistry of trace elemont uptako by some low Soaland bivalves. Limno.Occanogr. 10: 521-5 ark, F. W. & W. C. Whoolor i on tuents of marine invertebrates. U. S. 1922. Ino Cool. Surv. Profess: Pap., 12h: 1-62 Cornec, E. 1. Spectrographic studies of the ash of marine plants. Compt. Rend. 168: 513-511 Drinnan, R. E. ervations on the accuulation of hoa y motals by shell- 1966. fish in the estuary of tho iramichi River, N. B. Manuscript Series,! sheries Research Board of Canada 1966) Coldberg. Edward D. 1965. concentrations in marine organisms. Roviow of trace olomer Puerto Rico Nucl. Contor. 535 pp. Hardy Harrict Louise 1966. icology of lead. Symposium on onvironmental lead contam¬ ination, Publ. No. 1140, U.S. Pub. Heatth Serv., Washington, D. C. (Mar., 1966) eries Houblou, W. F., J. W. Wood, & E. R. Je. The toricity of zinc or cadmium for Chinook Salmon. Oregon 1. sheries comission Briefs 5:(1): ad insoly, ganese in modern and fossilized gastropod shells. ature,. 1959. (11 Mar. 1959) London 183: 170-171 cFarren, Earl Frances, James Edward Campboll & J. B. Engle Te occurrence of copper and zinc in shellfish. Proc., hth Sanit.! Shellf kshp., U. S. Pub. Health Serv., Append. R., p.2 Nicholls, Geoffrey Dennis, H. Curl, & V. T. Bowen Spectrographic analysis of marine plankton. Limnol. Occanogr. 172-178 1. auster, Carl Nathanial, Jr., & Bo jamin H. Pringle 1968. Effects of trace motals on ostuarine molluscs. Proc. Ist Mid¬ Atlantic Industrial Waste Conf,, Univ. Delaware, CE-5: 285-30h Vinogradov, A. P. 53. The elomontary chemical composition of marine organiams. Yale 640 pp. Univ., Now Haven, Conn. (Sears Found. for Mar. Rescarch) 21