HAZARD ASSESSMENT FOR CHLORINATED PARAFFINS: EFFECTS ON FISH AND WILDLIFE Health and Environmental Review Division Environmental Effects Branch Toxicology Branch January, 1985 ------- PRELIMINARY HAZARD ASSESSMENT ON. CHLORINATED PARAFFINS Executive Summary The following hazard assessment on chlorinated paraffins is based on the testing data submitted by the Chlorinated Paraffins Consortium in response to the negotiated testing as published in the Federal Register on January 8, 1982. o Results from the Phase I 60-day toxicity tests on rainbow trout and mussels indicate that the 58% chlorinated short chain length (Cio_i2) y* n-paraffins is the most toxic of the four formulations tested. o The Phase I testing matrix failed to adequately identify toxicological relationships between the wide array of chlorinated paraffin mixtures which vary both in the degree of chlorination and in the length of the carbon chain. o Results of the Phase II life-cycle studies on a variety of test species ^indicate statistically significant (P £ 0.05) toxic effects at measured concentrations of less than 10 ug/1 for sheepshead minnow, daphnids, and mussels, and at less than 20 ug/1 for rainbow trout, mysid shrimp, and a marine alga. - o Chronic effects of the 58% chlorinated short chain length n-paraffins ^ include abnormal behavior, growth effects, reduced reproduction, and lethality. o The extent of the effects and the maximum acceptable toxicant concen- trations (MATC) for most studies are obscured by shortcomings and erratic test results resulting from either poor testing procedures or husbandry problems. Adverse effects appear at test concentrations as low as 2.4 ug/1 and the results of adequate studies might indicate significant adverse chronic effects below 1 ug/1. o Studies on rainbow trout and mussels indicate extremely high levels of bioconcentration in both species for the 58% chlorinated short chain ------- length paraffins. The potential for bioconcentration of 'other chlorin- ated paraffins is indicated by the results of both the Phase I tests and published data. o Additional testing is necessary on other chlorinated paraffin fornula- tions to determine the extent of their toxicity and bioconcentration potential. o Test results of the Avian Reproduction Study indicate no significant effects on mallard ducks fed 28 and 166 ppm 58 percent chlorinated short chain length (Cio-12) n-paraffins. Significant effects reported at 1000 ppm include: 1) statistically significant decrease in eggshell thickness, and 2) a slight reduction in the percent of viable embryos per egg set, which was statistically significant for Weeks 3 and 6 only. ------- PRELIMINARY HAZARD ASSESSMENT CM CHLORINATED PARAFFINS The following hazard assessment on chlorinated paraffins is based on the testing data submitted by the Chlorinated Paraffins Consortium in response to the negotiated testing as published in the Federal Register on January 8, 1982. The testing agreement involved a two tiered testing scheme with Phase I tests conducted on four representative compounds selected from a matrix (Table 1). Phase II testing on additional aquatic species would be conducted on the most toxic of the four compounds. As seen from the Phase I test results presented in Table 2 for rainbow trout (Salmo gairdneri) and mussels (Mytilus edulis), the 58% chlorinated short carbon chain (Cio-i2) length paraffin was identified as the test material for the Phase II aquatic tests. This hazard assessment includes the results from the nineteen ecotoxicity studies (8 Phase I and 11 Phase II) submitted by the consortium and an avian reproduction study submitted by American members of the Consortium. Table 1 indicates what tests have been received and validated by OTS. The Avian Study and the Reproductive Study on ducks refer to the same test. The format followed in presenting the hazard assessment is as follows: each section begins with a discussion of the test results as submitted by the consortium, followed by a comparison of the results to information found in the published literature. For consistency, all test concentrations and their effect levels cited in this assessment are measured concentrations, since in many tests the measured concentration is considerably less than the nominal level. The summary at the end of each section is an assessment ofthe import- ance of the data and its potential impact on fish and wildlife. Due to the large number of complex studies, the strengths and weaknesses have been summarized, but not discussed in detail in this document under the Section titled - Adequacy of Test Data. A detailed description of the weaknesses and the validation for each study are available upon request. ------- 2 Acute Toxicity The only chlorinated paraffin for which acute studies were submitted is the 58% chlorinated short chain (€10-12) length n-paraffin. The acute aquatic LC50/EC50 values for this chlorinated paraffin range from less than 14.1 ug/1 to greater than 162 ug/1 (Appendix). High acute toxicity was reported in organisms from three of the six taxonomic groups. The three acutely sensitive species included mysid shrimp (Mysidopsis bahia), 96-hour LC50 < 14.1 ug/1; marine alga (Skeletonema costatum), 48-hour EC50 31.6 ug/1; and the waterflea (Daphnia magna), 48-hour LC50 about 46 ug/1. The 48-hour EC50 value of 530 ug/1 reported for daphnid is considered excessively high based on the mortality data reported during the chronic study. From mortality data on Day 2 reported in the chronic study, the LC50 could be estimated as about 46 ug/1. F Many researchers have reported low acute toxicity fpr fish for chlorinated paraffins. Johnson and Finley (1980) reported 96-hour LC50 values in excess of 300 nvg/1 for a series of static tests for various chlorinated paraffins to rainbow trout (Salmo gairdneri) and bluegill sunfish (Depends macrochirus) (Table 3). Acute data on channel catfish (Ictalurus punctatus) and fathead minnow (Pimephales promelas) also indicated low toxicity (greater than 300 and 100 mg/1, respectively). Variations in test temperature between 5° and 25°C did not reduce the static toxicity of Chlorowax 500C below a 96-hour of 300 mg/1. However, in flow-through tests with rainbow trout, sublethal effects were noted at concentrations as low as 40 ug/1. The effects primarily involved a progressive loss of motor function to the point of immobilization after 15 and 20 days of exposure. Death, when it occurred, resulted from debilitation and other secondary effects. These sublethal effects were not present or slightly expressed in bluegills and channel catfish. Madeley and Birtley (1980) exposed rainbow trout to Cereclor 42 (C20-30 42 * cl w/w) for 96 hours at 15°C. No mortality or abnormal behavior was noted at a mean measured level ------- 3 of 770 mg/1 (range 520-1630 mg/1). Linden et al. (1979) also tested several chlorinated paraffins on bleaks (Albumus alburnus), a European cyprinid minnow found in brackish water. Again, the 96-hour LC50 toxicity levels were low, greater than 5000 or 10,000 mg/1 at 10°C (Table 4). Recent tests with the harpacticoid copepod Nitocra spinipes have resulted in 96-hour LC50 values below 1 mg/1 (Tarkpea et al., 1981) for several chlorin- ated paraffin formulations having short carbon chains (<_ Ci7). These results summarized in Bengtsson and Ofstad (1982), were unavailable. As a result, the toxicity levels and identity of the tested chloroparaffins are unknown. The acute LD50 data on laboratory mammals as summarized by Howard et al. (1975) are greater than 10 gAg (Table 5). Acute LD50 and subacute LC50 data on mallard ducks (Anas platyrynchos) and the ring-necked pheasant (Phasianus colchicus) indicate that the chlorinated paraffin, Cereclor S52 (€14-17 an<^ 52% chlorination), is not acutely or subacutely toxic to birds (Table 6). While low acute toxicity of chlorinated paraffins has been indicated for ^ fish, tests with 58% chlorinated short chain length (Cio-12^ n-paraffins have shown high acute toxicity to roost tested aquatic invertebrates. High acute toxicity of other formulations is indicated in aquatic tests in which there are acute LCso values of less than 1 mg/1 for copepods, but the information on the identity of the tested formulations is not yet available. No toxicity informa- tion is available on sensitive test species identified in Consortium studies for formulations other than the 58% chlorinated short carbon chain (Cio_i2) length n-paraffins. Furthermore, the importance of a conclusion about low acute fish toxicity of chlorinated paraffins must be tempered by the extraordi- narily chronic nature of these chemicals. Mortality that begins in an acute test continues during longer exposures. For example, the 48-hour daphnid LCSO value was reported as 530 ug/1, while chronic test data indicate an incipient 6-day LCSO value of greater than 8.9 ug/1 and less than 16.3 ug/1. The chronic ------- 4 data also indicate a 48-hour LC50 value of about 46 ug/1. When the chronic daphnid LC50 values are plotted versus time, a near perfect chronicity curve is produced (Figure 1). Perfect chronicity is indicated when "effect concen- tration x time" yields a constant value. Chronic data on mysid shrimp also indicate some chronicity. Available chronic toxicity tests indicate that initial mortality is slow developing in some species and may even occur after the organism has been removed from the exposure. Thus, acute toxicity results may greatly underestimate the hazard of chlorinated paraffin formulations. r The low solubility of chlorinated paraffins in water raiseda few questions A concerning the validity of some of the high LC50 values reported in the litera- ture. None of the published articles indicated whether the test material was fully dissolved or even which, if any, solvent was used. High levels of test material added to water may underestimate the toxicity of a chemical, unless an organism is exposed to a toxicant which is either dissolved or dispersed into small enough particles as to be available. Since the literature contains mostly low acute fish toxicity values and no data on the more sensitive species identified in the Consortium studies, some concern for the more sensitive species remains for all formulations. High acute toxicity reported in copepods for several formulations indicate that not all formulations are of low acute toxicity. Given a propensity for chronicity, low water solubility, and the persistent nature of these chlorinated paraffins, the significance of acute values are of limited importance and chronic effects and incipient ££50 values should generally be considered more important to naturally occurring populations than acute toxicity. Chronic Aquatic Toxicity - Consortium Studies Chronic effects were reported in all test species for most all chlorinated paraffin formulations tested. The chronic effects include chronic mortality, significantly (P = 0.05) increased and/or reduced growth, abnormal behavior, ------- 5 reduced filtration (feeding) activity, reduced offspring per female, offspring mortality, reduced hatchability, reduced insect emergence, and reduced cell growth in algae. The maximum acceptable toxicant concentration (MATC) levels for these effects ranged as low as > 2.4 < 4.1 ug/1 and < 3.2 ug/1. The most sensitive species were sheepshead minnow larvae, mussels, daphnids, rainbow trout, mysid shrimp, and marine algae. All had no effect levels below 20 ug/1. The results from the Phase I, 60-day toxicity tests on mussels and rainbow trout exposed to four select chlorinated paraffin formulations, indicate that the greatest chronic toxicity occurred from the 58% chlorinated short chain (Cio-12) Ien9th n-paraffins (Table 2). The short chain paraffin with 58% chlorination shows greater hazard potential based on all of the criteria measured: abnormal behavior, mortality, and bioconcentration factor (BCF), compared to the results of the other three formulations. With the exception of the short chain length paraffins, mortality reported in the intermediate chain length (C^-ig) paraffin (52% chlorination) and long chain length (€20-30) paraffins of low (43%) and high (70%) chlorination was 7 percent or less for all test levels and abnormal behavior in rainbow trout was either equivalent to controls or transient on Days 5, 8, and 9. Abnormal behavior in mussels was reported as reduced filtration (feeding) activity and generally occurred only at highest test concentration. Patterns of toxicity related to carbon chain length and/or percent chlorination could not be found, because the test concen- trations were too low to yield effect levels for most studies. ./ Chronic effects of short chain length paraffins on mussels include chronic mortality, reduction in shell and tissue growth, and reduction in filtration (feeding) activity. Continual mortality throughout the test period produced a 60-day LC50 value of 74 (68 - 81) ug/1. Mortality at 13 ug/1 (0 percent) and 44 ug/1 (2 percent) are insignificant. Non-quantitative observations were made on filtration and effects were reported on a number of occasions at 13 ug/1, ------- 6 the lowest test concentration. Significant (P'£ 0.05) reduction in the rate of growth was reported in the growth effects study oh the 58% chlorinated short chain length paraffins for both tissue weight and shell length." Both growth rates were reduced 53 percent and gave a MATC of greater than 2.3 ug/1 and less than 9.3 ug/1. Estimation of growth rates from Phase I 60-day, toxicity data indicate values too small (0.2 - 2 percent) for comparison. Growth in Phase I studies were lower than normal, because the mussels had been fed a diet suffi- cient only for maintenance and not enough to support vigorous growth. Chronic effects of short chain length paraffins on juvenile rainbow trout include chronic mortality, abnormal behavior, and growth effects. Chronic lethality occurred throughout the test period of 60 days with 33 percent death at concentrations as low as 33 ug/1. Abnormal behavior in fish was reported as persistent and slight to moderate at the lowest observed test level (33 ug/1). The growth study reported significant (P £ 0.05) growth effects at > 3.4 ug/1 < 17.2 ug/1 (26 percent increase in weight). If the subsample weights are assumed representative in each test group, increased growth was also evident at 33 and 100 ug/1, while growth reductions occurred at test levels greater than 350 ug/1 and less than 1,070 ug/1 (Table 7). The MATC reported for the study is greater than 3.4 ug/1 and less than 17.2 ug/1 based on growth effects. Study One on sheepshead minnow embyro-larvae indicates chronic effects including significantly (P £ 0.05) increased growth levels at all test levels (2.4 - 55 ug/1) for length and at all concentrations greater than 2.4 ug/1 and s less than 4.1 ug/1 through 55 ug/1 for weight. Growth levels for length and weight in the second study were significantly increased at 36 and 71 ug/1 and significantly reduced at 620 ug/1 (Table 7). The degree to which the toxicant affected larval growth is partially obscured by the reduction in growth caused by acetone, compared to controls. In the first study, length was significantly (P £ 0.05) reduced 4.3 percent in acetone controls. Length reduction of 8.5 ------- 7 * percent in the second study, although larger was not statistically significant. In the same studies weight in the acetone controls were reduced by 5.9 and 16.9 percent, but neither value was statistically significant. The effect of acetone reductions on growth would be to overestimate increased growth and underestimate growth reductions. No significant effect was found on sheepshead minnow hatch- ability or larval survival at test levels as high as 620 ug/1. Reproductive effects on daphnids were obscured by high variability in the test results and non-dose-related effects. One pair of replicate controls produced 52 percent fewer offspring compared to the other control. The lowest test level (2.7 ug/1) produced 44 percent fewer offspring compared to acetone controls, while 5.0 ug/1 produced only 16.4 percent fewer offspring and the highest concentration (8.9 ug/1) produced 66 percent fewer. While none of the > results are statistically significant (P £ 0.05), differences between treatment groups are apparent. The effect at the highest test level appears to be at least partially due to the toxicant, but the degree of effect can not be ascertained. Differences in parental length followed the same erratic effect pattern seen in the production of offspring. The description of the test vessel positions and similarity between results for each repetition, especially between the two sets of controls, provide strong evidence to support the hypo- thesis that the erratic results are due to the position of the test vessels and not primarily due to the toxicant. In the flow-through chronic study, the insipient daphnid LC50 value of greater than 8.9 ug/1 and less than 16.3 ug/1 ,s was attained by Day 6 and remained unchanged through Day 21. The semi-static chronic test produced similar mortality levels with 50 percent mortality at 12.0 ug/1 from Day 7 to Day 14 and no deaths at 6.3 ug/1. No mortality occurred in the static test before Day 5. Chronic effects on mysid shrimp include chronic mortality, which may be sex-related, and a possible reduction in reproduction. First generation deaths ------- 8 began on Day 2, crested on Day 21, and continued throughout the 28-day test. Parental mortalities seemed to be sex-related with 77 percent of the deaths being male. Unfortunately, the chronic mortality among parents"was not dose- related. While some chronic mortality reported in the mysid study might have been due to the test material, the effect levels on reproduction were obscured apparently by husbandry problems. These husbandry problems also appeared to affect the number of young per female which were too variable to identify significant effects. The reduction in young per female at 7.3 ppb, compared to acetone controls (7.46 versus 11.07 young/female, respectively), would appear to be due to chlorinated paraffin toxicity. The resultant MATC for mysid shrimp probably should be greater than 3.8 ug/1 and less than 7.3 ug/1. Chronic effects in chironomid midges exposed to 58% chlorinated short chain length (Cio-12^ n-paraffins include reduced hatching in Gj parental egg masses, no emergence of adults, and reduction in the number of eggs per egg mass. Hatching of midge larve from parental egg masses was reduced 60 percent at test concentrations of 78 ug/1 compared to controls. At concentrations of 121 and 162 ug/1, there was no emergence of first generation adult midges. At 78 ug/1, the highest test level yeilding young, the number of second generation eggs per mass was reduced 10 percent, but that was not significantly (P _< 0.05) different than controls. Behavioral effects were reported in a number of the Consortium studies on mussels and rainbow trout. Abnormal behavioral effects in mussels were reported in test concentrations for all formulations tested in Phase I. The unquantified behavioral observations reported were reduced filtration (feeding) activity. The frequency and intensity of the effect corresponded directly to the test concentration and generally corresponded conversely to carbon chain length and the degree of chlorination (Table 2). Behavioral effects were also evident as reduced growth in all of the mussel studies tested with 58% chlorinated short ------- 9 chain paraffins. In the Phase I study, the reduced filter-feeding activity was observed on a number of occasions at 18 and 56 ug/1, but caused no nortality. Significant mortality (over 50 percent) followed abnormal behavior at 71, 130, and 930 ug/1. No behavioral observations were reported in the growth or bioconcentration studies, but adverse effects were indicated in both studies. In the growth study, a significant reduction in shell and tissue growth was reported at 9.3 ug/1, which would be expected from reduced feeding activity. In the bioconcentration study, 33 percent mortality was reported at 10.1 ug/1 (23% during the exposure phase and 10% during depuration). Deaths at 2.35 ug/1 were not significantly higher than controls. In the 60-day Phase I test on rainbow trout exposed to 58% chlorinated short chain paraffins, abnormal behavior began on Days 2 and 3 for all tests levels and showed a dose-related response. The lowest test level (33 ug/1) affected occasional individuals and deaths began on Day 11 (33 percent by the end of the study). The highest test level (3,050 ug/1) consistently affected behavior in over half of the fish after Day 14 with the first deaths occurring on Day 9. The smaller fish appeared to be affected first in any test group and subsequently their symptoms were usually more severe. Symptoms proceeding death followed a regular pattern which began with a slow response to food and eventually to not feeding at all, next came lethargic behavior, an apparent inability to change position within a depth in the aquarium, long periods on the bottom, darkening of skin pigmentation, occasional periods of activity ** without direction, infrequent tetanic spasms, and death within 5 to 15 days after establishment of symptoms in an individual. Starvation was suggested as possibly contributing to eventual death. While fish behavior appeared normal in the growth study and no significant mortality occurred, the bioconcentration study indicated significant dose-related mortality. While only three deaths occurred about two-thirds of the way through the exposure phase, a total of ------- 10 thirteen fish died beginning on Day 64 through'Day 69 of the depuration phase. All fish which had been exposed to the higher test level, 14.3 ug/1, died 36 days before the final sampling date. Only two fish survived afthe 3.1 ug/1 test level. The authors indicated that these deaths were proceeded by symptoms * of abnomal behavior reminiscent of those described in the 60-day toxicty study. No behavioral observations were made in the sheepshead minnow studies and no significant larval mortality occurred. Chronic Wildlife Toxicity - American Manufacturers The mallard reproduction study indicate no significant effects from diets of 28 and 166 ppm 58% chlorinated short chain length (Cio-12^ n-paraffins. The statistically significant effects identified in mallards fed 1000 ppm include: 1) a decrease in eggshell thickness of 0.02 mm (mean 0.355 mm versus 0.375 mm in controls), and 2) slight reduction in the percent of viable embryos per egg set (85% versus 95% in controls), which were statistically significant only for Weeks 3 and 6. While eggshell thinning was statistically significantyreduced \-f in the group fed 1000 ppm, the thickness falls within levels which the protocol considers acceptable for for controls. The statistically significant decrease in adult food consumption at 28 ppm during Week 17 should be considered to be spurious and unrelated to toxicological effects. All other reproductive parameters analyzed statistically showed no significant differences from the controls and control reproductive parameters were within acceptable levels. Chronic Toxicity - Published Literature Many publications have reported chronic effects on test organisms from exposure to chlorinated paraffins. Johnson was the first to find neurotoxic effects on fish behavior following chronic exposure to chlorinated paraffins. The results of the flow-though tests on rainbow trout were later reported in Johnson and Finley (1980). Sublethal effects were seen at concentrations as low as 40 ppb and included progressive loss of motor function to the point of ------- ' 11 immobilization after 15 and 20 days. Death, when it occurred, resulted from debilitation and other secondary effects. These sublethal effects were not seen or only slightly evident in bluegill and channel catfish. No significant differences in susceptibility were found between yolk-sac fry, swim-up fry, and fingerlings in. tests on rainbow trout. Svanberg et ad. (1978) reported obvious signs of neurotoxic effects in adult bleaks which first became apparent after exposure for 14 days at 1 mg/1, the high dose, and later at the low dose (0.1 mg/1) of Chlorparaffin Huls 70 C (short chain, 70% chlorination). Symptoms were similar to other studies and included sluggish movements, disturbed orientation in the aquarium, tetanic spasms, and death. The three deaths (7 fish/level) occurred on Days 15, 28, and 27 at exposure levels of 0.1, 0.1, and 1.0 mg/1, respectively. Residues in the three dead fish were 20.3, 32.8, and 47.5 ug/g, respectively. Live fish residues reported on Day 29 in the same test were 26.2 and 28.6 ugCl/g at exposures of 0.1 and 1.0 mg/1, respectively. While data reported by Svanberg et^ al. indicate that the residues in dead fish were generally higher than in live fish, insufficient data were available to confirm this observation or to establish lethal body residue levels. Bengtsson et cd. (1979) reported sluggish movements, absence of shoaling behavior, and abnormal vertical positions after 7 days exposed to 125 ug/1 of Witaclor 149, 159, and 171P in decreasing order of pronounced effects. No abnormal behavioral effects were reported for Witaclor 350, 549, and the PCB, s Clophen A50, during the 14-day exposure. Several published studies indicate similar neurotoxic symptoms in fish following dietary exposures to chlorinated paraffins. Bengtsson and Ofstad (1982) fed several chlorinated paraffins to bleaks and reported the following behavioral effects. The first changed behavior was noted in the Witaclor 149 high dose group (5800 ug/g of 49% chlorinated Cio-13 paraffins) after 5 weeks ------- 12 exposure. Symptoms included sluggish swiinming closer to the bottom than usual. After 7 and 12 weeks, the same behavior was seen in the Witaclor 149 medium dose group (2500 ug/g) and the Witaclor 171P group (3180 ug/g of 70% chlorin- ated Cio-13 paraffins), respectively. This behavior was generally accompanied by folded dorsal fins and minor balance problems. The effects gradually disappeared within a couple of weeks during the subsequent depuration period. Evidence of chronic lethality of chlorinated paraffins had previously been reported by Zitko (1974) in contaminated food uptake tests on juvenile Atlantic salmon. While the differences in mean time to lethality (LT50) are evident between the control and both chlorinated paraffins test levels, an inversion in the LT50 data is apparent between 10 and 100 ug/g Cereclor 42 (Table 8). Insufficient information was given to identify the source of the LT50 inversion, but reduced feeding at the 100 ug/g concentration which was neither measured nor reported could easily be responsible for such a toxicity inversion. In tests where fingerling rainbow trout were fed a diet fortified with 10 ppm Chlorowax 500C (X C\2 an^ 60% chlorination) for 82 days, growth was reduced in treated fish, but they showed no gross pathological effects (Lombardo et_ al.f 1975). Significant chronic effects reported on 58% chlorinated short chain length n-paraffins include chronic mortality in most species, dose-related increases and reduction in rainbow trout and sheepshead minnow growth, growth reduction in mussels, reduced adult chironomid emergence, reduced reproduction in mysid shrimp and daphnids, and possibly sex-related lethality in mysid shrimp. While chronic exposures in Phase I testing on other formulations failed to produce significant mortality, abnormal behavioral effects were reported in mussels and rainbow trout. These behavioral effects are especially evident for all formulations in the form of reduced filtration (feeding) activity in mussels. Adverse effects, other than mortality, were most apparent in sensitive test ------- 13 species which were tested only with the 58% short chain length paraffins. Mortality and neurotoxic effects have been reported in fish studies following both aqueous and dietary exposures to several chlorinated paraffins. The appearance of synpterns are sequential and are similar over a wide range of formulations. Comparative Toxicity Significant growth effects present in rainbow trout and sheepshead minnow show a similar pattern of significant increases at low test levels and signifi- cant reductions at high test concentrations. The test concentrations at which the growth effects are found are nearly the same for both species (Figure 2). Similarity in the growth curves for the two species strengthens the validity of the unusual dose-response to a test substance. The mechanism responsible for increased growth at low test levels is not understood, pifferenoes in rainbow trout mortality in the bioconcentration and growth studies tested at similar concentrations and exposed for 168 days each are not clear. Two possible sources for the mortality difference are duration of observation period and higher levels of chlorinated paraffin contamination in the fish food (2.2 ppm versus 0.8 ppm) in the bioconcentration study. An estimate of the residue contribution from water and from food indicates that at the higher test levels, about 15 ug/1, the food contribution would have been only about 2 percent of the total body residue and therefore, insignificant compared to the exposure from water. At the lower test level, about 3.0 ug/1, contaminated s food would have contributed about 30 percent. Analysis of the mortality data showed that the significant mortality occurred during the depuration phase 64 to 69 days after the 168 day exposure had ceased. The timing of the deaths and the fact that 80 percent of the whole body residues had been eliminated at the time of death, indicate that the duration of the observation period might best account for the discrepancy in the mortalities. Absence of toxicant- ------- 14 related mortality in sheepshead minnow larvae exposed 32 days at test levels through 620 ug/1, a concentration level greater than which killed most rainbow trout in the 60-day toxicity test, also supports the concept that mortality differences might be time related. Significant differences in susceptibility are not found either among various earlylife stages in rainbow trout or sheeps- head minnow. Some species differences in sensitivity to chlorinated paraffins are indicated by the occurrence of only slight or no sublethal effects in bluegills and channel catfish compared to effects reported on rainbow trout. Growth studies on mussels exposed to the same short-chained length chlor- inated paraffin indicate reduced growth rates at concentrations greater than 2.3 ug/1 and less than 9.8 ug/1 (53 percent reduction in both tissue and shell length). Toxicant levels reducing mussel growth are less than the concentra- tions reported to reduce growth in sheepshead minnow (greater than 280 ug/1 and less than 620 ug/1) and in rainbow trout (greater than 350 ug/1 and less than 1,070 ug/1). Daphnids and mysid shrimp are both affected by the 58% chlorinated short chain length paraffin at similar concentrations. The 96-hour LC50 values are 18 ug/1 and less than 14 ug/1, respectively. The number of daphnid offspring per female is reduced 44 percent at 2.7 ug/1, the lowest test concentration, versus a 33 percent reduction in offspring/female in mysid shrimp at 7.3 ug/1. Chironomid midges, another aquatic invertebrate, are not as sensitive as the above two invertebrates, but adverse reproductive effects on midge larvae were ^ reported for hatching, emergence, and eggs per mass at concentrations of either 78 or 121 ug/1. The two species of algae reacted very differently when acutely exposed to 58% chlorinated short chain length n-paraffins. The marine alga, Skeletonema costatum, was the more sensitive species with a 96-hour EC50 of 42.3 (27.3 - 93.1) ug/1 for growth (cell count). The effect of the test material on growth ------- 15 * rate of the marine alga was however transitional and by Day 10 no difference in growth rates were apparent when compared to controls (Figure 3). The highest reduction in growth rate occurred during the first two days and produced 48-hr EC50 of 31.6 (20.7 - 57.6) ug/1. Toxicant effects on the freshwater green alga, Selenastrum capricornutum, differed from the marine alga in that growth rate reduction was produced by higher test concentrations and the greatest effect occurred at the end of the 10-day study rather than in the first few days (Figure 4). The lowest reported EC50 for the green alga was 1,310 (880 - 4,060) ug/1 at 10 days, which was derived by extrapolation from the 45 percent reduction found at the highest test level, 1,200 ug/1. Increasing differences in growth rates compared to controls in the latter days of the study indicate that longer exposure would probably produce lower effect levels for green alga. How much lower is unknown. Physical Test Factors Affecting Toxicity Adverse effects due to458% chlorinated short chain length paraffins are evident across a wide array of taxonomic groups tested. Significant (P <_ 0.05) effects occurred in a range of about 2.4 to 20 ug/1 for most species including both fish species, the mussel, daphnids, mysid shrimp, and one of the two algae species tested. No toxicity pattern could be found between species found in marine or freshwater or between species tested at high or low temperatures. The two major factors affecting the toxicity of chlorinated paraffins appear to be time and concentration. While the influence of the test concentration is ^ an obvious factor, the duration of the test period to the extent necessary to show toxicity as is the case in the chlorinated paraffins is unusual. As seen above, the duration of the exposure (168 days) and an additional 64 to 69 days of post-exposure observation passed before significant mortality occurred in the bioconcentration study. Very few chemicals show such prolonged developing, chronic effects, and even fewer demonstrate delayed mortality so late into the ------- 16 * depuration phase. While some fish species are iriore sensitive to chlorinated paraffins than others, no toxicological pattern could be identified. Little information is available from which the extent of chronic effects may be determined for the other chlorinated paraffin formulations. The 60-day toxicity studies reveal no significant chronic mortality, and the sublethal chronic observations were not quantified. The occurrence of sublethal effects is indicated by some reported, but unquantified, abnormal behavior, especially the reduction of filtration (feeding) activity seen in the mussels. Neurotoxic effects reported for rainbow trout and bleaks include a similar reduction in feeding activity described as a slowed response to food. The results of growth studies on mussels, rainbow trout, sheepshead minnow, and bleaks indicate reductions in growth, which most likely result from reduced feeding. Abnormal behavior has been reported in bleaks for other formulations of chlorinated paraffins, especially for the shorter carbon chain lengths of all levels of chlorination. Abnormal behavioral effects are greater for the 49% chlorinated formulation than for 59% chlorination, which in turn is greater than for 71% chlorination. Aquatic Bioconcentration and Bioaccumulation Long-term bioconcentration studies on mussels and rainbow trout exposed to 58% chlorinated short chain length paraffins demonstrated high BCF levels in whole organisms ranging from 24,800 to 40,900 and 3,550 to 5,260, respectively. While the data for some organs were erratic and never stabilized, equilibrium ^ between water concentrations and whole organism residue levels were reached in about 45 to 80 days in the mussel and by about Day 90 in the rainbow trout. Depuration half-life rates for the whole organisms were reported as 9.2 to 19.8 days in the mussel and 18.7 to 19.8 days in the rainbow trout. Of the tissues measured the highest residues occurred in the digestive organs of both species. BCF levels in the mussel's digestive gland/stomach ranged from 104,000 to ------- 17 226,000. In the rainbow trout, initial residue levels were highest in the liver and viscera with BCF values of 11,430 to 15,970, but the levels in the liver declined in the latter half of the study to 2,770 to 3,930. BCF values found in flesh or carcass were considerably lower (1,330 to 5,040). Declining residues in the trout liver give the impression that active elimination of Cl4, possibly occurs via metabolic breakdown of the chlorinated paraffin. The bioconcentration study on mussels exposed to nominal concentrations of 2.35 and 10.1 ug/1 of 58% chlorinated short chain paraffins indicate BCF values of 40,900 and 24,800, respectively for the whole animal. Compared to the gonad and residual tissues, the digestive gland had the highest residue levels with BCF values of 104,000 and 226,400 at levels of 2.35 and 10.1 ug/1, respectively. Whole animal residues attained equilibrium at the highest exposure level at about Day 42, which also corresponded to the onset of low level mortality that persisted throughout the 91-day exposure and through Day 125 (34 days into the depuration period). As discussed earlier, mortality also occurred in the rainbow trout bioconcentration study during the depuration phase. However the trout deaths began after 64 days of elimination and ceased on Day 69, leaving only two surviving fish at the lowest test level. As indicated above, the contamination of the fish food source at 2.2 ppm is not considered responsible for this late mortality during the depuration phase. Additional data on bioconcentration are available from the Phase I, 60-day toxicity tests, but the results must be considered preliminary, because the ^ studies did not follow OTS-recommended protocols. The two major deficiencies in the 60-day studies are that only one sample per treatment level was made and the test organisms were fed a maintainenoe diet rather than a diet adequate for growth and deposition of body fat. The BCF value reported for each exposure level provides a single data point at 60 days with no indication of either sample variability or the maximum bioconcentration level. For most chemicals, ------- 18 60-days exposure would be expected to be sufficient to reach equilibrium, but for the chlorinated paraffin formulations that duration has not been shown to be adequate. The effect of a minimal diet level necessary to maintain body functions on bioconcentration is uncertain. The preliminary BCF levels reported in all mussel studies may be underestimated, because the mussels were fed a maintenance diet which limited growth and the deposition of additional lipids where chlorinated paraffins would be stored. The growth rate in the 60-day mussel tests was only 0.2 to 2 percent compared to growth of about 30 percent for the same time period in the mussel growth study. Frequently, chemicals are bioconcentrated and deposited in fatty tissue and lipids more effectively when the organism is actively growing. As a result of the above deficiencies, the BCF values reported in the 60-day tests may be used, but must be considered preliminary and are an indiction of the minimum BCF level for each tested formulation. The BCF values reported in the two bioconcentration studies agree well with the results reported on the same test material in the 60-day toxicity tests submitted on the mussel and rainbow trout. The preliminary BCF values for the other chlorinated paraffin formulations with different carbon chain lengths and degrees of chlorination reported in the 60-day toxicity tests also indicate a propensity for bioconcentration. The preliminary bioconcentration rates in both species appear to decrease with increasing chain length (Table 2). The differences in the preliminary BCF between the low (43 percent) and s high (70 percent) chlorinated long chain paraffins are too small to draw any conclusion about the effect of chlorination levels on BCF. The BCF values reported in the mussel and rainbow trout bioconcentration tests are consider- ably higher than chlorinated paraffin values previously reported in the liter- ature (Table 9), but in close agreement with BCF levels reported for the same mussel species exposed to DDT (4,550-49,600) and PCB (7,200-26,600) by Geyer et ------- 19 al. (1982). Svanberg et al. (1978) exceed bleaks to 0.1 and 1.0 ppm of Huls Chlor- paraffin 70C (X GH.S and 70% CD which resulted in BCF levels"of 28.5 - 328 X after 29 days exposure. Bengtssen et al. (1979) exposed fish to several chlor- inated paraffins for 14 days followed by an elimination period of 7 days. While their BCF values ranged from 32 to 760 X, the pattern of decreasing bioconcentration rates with increasing chain length and increasing percent chlorination is evident (Table 6). Residue levels after 7-days depuration indicate residue losses of less than 50 percent for all formulations, except the PCB formulation. Zitko (1974) compared the level of accumulation of Cereclor 42 (42% CD, Chlorez 700 (70% CD, and PCB, Aroclor 1254 (54% CD in juvenile Atlantic salmon (Salmo salar) exposed via two sources, uptake of chlorinated paraffins in suspended solids (1 g/1 of contaminated silica) for six days (Table 9) or over 181 days in dry fish food at levels of 10 and 100 ug/g (Table 10). The BCF level could not be calculated in either case, because data on the level of exposure is missing for both exposures. Although the test period was consider- ably shorter, residue levels were higher from exposure to the suspended contam- inated silica particles as opposed to consumption in the food. Several other authors also reported residues in fish following dietary exposures to various formulations. Lombardo et al. (1975) fed rainbow trout a diet with 10 ppm of Chlorowax 500C (X Ci2 and 60 % CD for 82 days. In the f> samples taken approximately every two weeks, chlorinated paraffin residues in body tissues (i.e., less head, tail, and viscera) measured only as high as 1.1 ppm. Analysis of the data indicate that a residue plateau was never attained and the rate of uptake never slowed even after 82 days. Bengtsson and Ofstad (1982) fed several chlorinated paraffin formulations mixed in food pellets to adult bleaks for a period of 91 days. Whole body, ------- 20 residue levels were measured periodically during the exposure and depuration periods (Table 10). Residues of short chain length, low chlorinated paraffin accumulated faster than the residues of the other two formulations. As might be expected, the residue levels in the fish correlate directly to the concen- tration in food, but the BCF values are inversely related to the dose level. Depuration is rapid, about a 92 percent residue loss in 7 days. The short chain, highly chlorinated and long chain length, low chlorinated paraffins accumulate residues in bleaks more slowly than the short chain, low chlorinated paraffins. Their depuration half-lives could not be calculated from the avail- able figure, but they were longer than the 316-day elimination period. A similar pattern of bioconcentration and depuration rates were reported in an earlier study, where bleaks were tested for shorter exposure periods in water (Bengtsson et al., 1979). Comparable data from the Consortium studies and from published literature indicate that bioconcentration and depuration rates for chlorinated paraffins are inversely related to carbon chain length and the degree of chlorination (Table 11). Comparison of residue bioconcentration rates from water and dietary exposures indicate that chlorinated paraffins are generally taken up more quickly from water than from food by bleaks and rainbow trout. Even when dietary levels are over 1000 times the water concentration, uptake rates from water are equal to or greater than from the diet (Figure 5). Uptake rates for long chain length or highly chlorinated paraffins from water and the diet are ^ similar, despite the 1000-fold difference in their concentrations. High levels of bioconcentration such as indicated by chlorinated paraffins is a concern to the well-being of the organism which stores it and to any other animal that would consume that organism. The stored chemical might adversely affect the organism during periods of stress, such as starvation, migration, and reproduction, or affect the developing offspring as a result of chemical ------- 21 residues stored in lipids of the egg. Bioconcentration is especially signifi- cant, because the residues usually also accumulate in those species highest on the food web and any adverse effect on them is accentuated by their typically low reporductive potential. Furthermore, mortality data in the mussel and rainbow trout bioconcentration studies indicate that adverse effects do not cease when exposure ends. Both species experienced mortality during the depur- ation phase. The mussel mortality at the higher test level began during the exposure period about Day 43 and occurred persistently 34 days after the depur- ation period started. Rainbow trout deaths began 64 days into the depuration period and within a week all died except two fish at the lower test level. The combination of high BCF values, slow depuration, high toxicity, persistence, and widespread distribution of these chlorinated paraffins in the environment are of considerable concern with respect to fish and wildlife safety. Terrestrial Bioconcentration and Bioaccumulation No bioconcentration data, per se, are available on chlorinated paraffins. £ Samples from muscle, fat, and eggs of mallards were frozen during the avian reproduction study, but no residue analyses on these tissues were made. In the literature, the distribution of chloroparaffin residues in quail and mice was investigated using autoradiography. Biessmann et al. (1982) gavaged Japanese quail with two chloroparaffins (Ci2 ~ 55.9% chlorination and Cig - 34.1% chlorination). Distribution of both chloroparaffins were nearly identical at each sampling. Shortly after dosing the highest radioactivity was found in s tissues with high metabolic activity and high cell turnover rates, and in the bile and urine. Tissues with strong labelling were: liver, intestinal mucosa, spleen, bone marrow, oviduct, gall bladder, kidney, yolk, eggshell, and, to a lesser, extent in the albumen. Later, the radioactivity was most evident in follicle yolk, uropygial gland, and fat. Residue levels of C^g were about twice that of Cj2 in the first 10 eggs laid after dosing. ------- 22 Darnerud and Brant (1982) found similar residue patterns in active tissues in mice following intravenous and oral doses with 34.1% chlorinated hexadecane (Cig). Marked uptake of radioactivity occurred in the brown fat, intestinal mucosa, bone marrow, and exocrine glands. All of these tissues have high rates of turnover and/or high metabolic capacity. No differences were found in the distribution of residues for oral or intravenous dosing with the exception of higher radiolabelling of the stomach and intestines in the orally-dosed mice. Biessmann et al. (1983) repeated the above tests on quail and mice using the same methods of administration with Cjg ~ 69% chlorination for comparison. Distributions of residues were similar to the results above, except that little l^COj was released indicating a different metabolic pathways. The formation of ^CC>2 and incorporation of radioactivity into metabolically active tissues are inversely related to the degree of chlorination. Darnerud et al. (1983) also studied residue distribution patterns in two fish species, carp and bleaks. The distribution of 34% chlorinated hexadecane (Cig) injected arterially into the fish was similar for the two species. Like the quail and mice, residues were found to concentrate in active tissues, such as kidneys, liver, nasal mucosa, and fat. Large amounts of radioactivity were also excreted in bile for both fish. Samples taken five days after injection also showed marked uptake in the gills, testis, and brain. After 13 days, the residue levels were generally lower, except for the comparably high residues seen in the liver. They concluded that the residues were incorporated in the ^ tissues and subsequently organically bound chlorine are retained for long time. Adequacy of Test Data Several major problem areas were recognized as pertinent to all or nearly all of the submitted studies. The reoccurring problems identified in these studies are of varying seriousness and have been submitted to the researchers for clarification, comment, and improved testing in future tests. ------- 23 f Additional Testing Needed Several of the tests were incomplete or inconclusive including all those tests submitted for which the test levels were too low to produce an observable effect. If the predicted environmental concentrations (PECs) used in the risk assessment are in the range of 0.1 to 100 ppb, some aquatic tests might have to be repeated in order to clearly quantify the adverse effects. The studies which may need to be retested on 58% chlorinated short chain length n-paraff ins include: 1) Daphnia magna life-cycle test 2) Mysid shrimp life-cycle test 3) Sheepshead minnow embryo-larvae test Other testing may be required, especially since the testing matrix has failed to provide adequate data points from which to interpolate the toxicity of all chloroparaff in formlations in the matrix based on percent chlorination and chain length. These toxicity data do not permit extrapolation to other chlorinated paraffin formulations. Phase II tests for each of the matrix group may be needed, unless an adequate new matrix can be constructed. Conclusions Phase I test results indicate that the 58% chlorinated short chain length n-paraff ins are more toxic than the other three tested chlorinated paraffin formulations. The matrix fails to indicate if it is the most toxic of all chlorinated paraffin formulations. While the short chain length paraf- ^ fins are more toxic, the other formulations are not without observed chronic effects. Unquantified abnormal behavior reported, especially upon mussel filtration (feeding) activity, indicates that chronic effects are probable in all formulations. Preliminary bioconcentration factors indicate that all four « formulations will accumulate. The extent of bioconcentration in the Phase I tests could not be asertained due to the inadequacy of the sampling methods, ------- 24 (i.e., tissue levels were measured at only one point in time with no assurance that these slowly accumulated chemicals had reach' equilibrium with levels in the water). Consequently, the BCF values reported for the tested formulations in Phase I tests must be considered preliminary and minimal values. Bioconcen- tration factors were determined in Phase II testing only for the 58% chlorinated short chain length paraffins. In rainbow trout and mussel studies, the BCF values were reported as 3,550-5,250 and 24,800-40,900, respectively. These levels of bioconoentration are of considerable concern, especially when combined with the persistence such as has been indicated for chlorinated paraffins. Residues may be expected to enter the aquatic environment and be found in most, if not all, organisms, especially those species at the top of the food web. Phase II chronic tests on 58% chlorinated short chain length n-paraffins indicate significant (P = 0.05) chronic adverse effects in the range of 2.4 to 20 ug/1 for rainbow trout, sheepshead minnow embryo-larvae, mussels, daphnids, mysid shrimp, and the marine alga. These effects generally include chronic lethality, altered growth, and reduced reproduction. Shortcomings identified in most of the studies preclude identifying the lowest effect level concentra- tion as well as the percent of the adverse effect. Analysis of the aquatic data indicate that adverse effects occur at the lowest concentration tested (2.4 ug/1) and that testing at lower levels may produce significant adverse effects below 1 ug/1. s Reproductive effects of 58% chlorinated short chain length n-paraffins on mallard ducks include statistically significant effects on eggshell thickness and percent viable embryos per egg set at 1000 ppm. The no observed effect level found in the avian reproductive test was 166 ppm. Distribution of chloroparaffin residues in tissues appear to be similar for species as diverse as mussels, fish, quail, and mice. Residues tend to ------- 25 accumulate in tissues with high cell turnover 'rates and/or a high metabolic capacity. Rates of C£>2 formation and levels of residue incorporation into metabolically active tissues appear to be inversely related to the degree of chlorination. Summary The chronic studies on the 58% chlorinated short chain paraffins indicate a concern for the well-being of aquatic organisms across a broad spectrum of taxonotiic groups at environmental levels of 2.4 to 20 ug/1. Adverse effects occur below that level into the parts per trillion range are indicated, but they can not be assessed due to the inadequacies in the studies identified above. Also, available data do not demonstrate that the most toxic chlorinated paraffin has been identified. The 60-day toxicity data on the other paraffin formulations are also insufficient to conclude that they have no adverse chronic effects. In fact, the unquantified observations of reduced filtration (feeding) activity reported in mussels indicate that effects on mussel growth are probable for all tested formulations. The breadth of toxic effects on a wide variety of species from various environments indicate that chlorinated paraffins pose a potential threat to a wide variety of aquatic species in freshwater, estuarine, and marine environments. Chloroparaffins are much less toxic to mammals and birds than to aquatic species. Acute toxicity to these two groups is virtually non-existent. Moderate chronic effects occur in avian reproduction. Avian reproductive s effects include statistically significant reductions in egg shell thickness and the percent of viable embyros per egg set at 1000 ppm (NOEL 166 ppm). Organically-bound chlorine residues appear to concentrate in tissues with high cell turnover rates and/or a high metabolic capacity. ------- Literature Cited Bengtsson, B.-E.f O. Svanberg, and E. Linden. 1979. Structure related uptake of chlorinated paraffins in bleaks (Alburnus alburnus). Ambio 8(2-3): 121-122. Bengtsson, B.-E. and E. B. Ofstad. 1982. Long-term studies on uptake and elimination of some chlorinated paraffins in the bleak, (Alburnus alburnus). Ambio 11(1):38-40. Biessman, A., I. Brandt, and P. 0. Darnerud. 1982. Comparative distribution and metabolism of two l^oiabeHecl chlorinated paraffins in Japanese quail Cotumix coturnix japonica. Environ. Poll. (Ser. A) 28(2):109-120. Biessman, A., P. O. Darnerud, and I. Brandt. 1982. Chlorinated paraffins: Deposition of a highly chlorinated polychlorohexadecane in mice and quail. Arch. Toxicol. 53(l):79-86. Birtley, R. D. N., D. M. Conning, J. W. Daniel, D. M. Ferguson, E. Longstaff, and A. A. B. Swan. 1980. The toxicological effects of chlorinated paraffins in mammals. Toxicol. Appl. Pharmacol. 54(3):514-525. Campbell, I. and G. McConnell. 1980. Chlorinated paraffins in the environment. 1. Environmental occurrence. Environ. Sci. Technol. 14(10):1209-1214. Darnerud, P. O., B.-E. Bengtsson, A. Bergman, and I. Brandt. 1983. Chlorinated paraffins: Disposition of a polychloro-[l-14c]-hexadecane in carp (Cyprinus carpio) and bleak (Alburnus alburnus). Toxicol. Lett. 19(3):345-351. Darnerud, P. O., A. Biessmann, and I. Brandt. 1982. Metabolic fate of chlorin- ated paraffins: Degree of chlorination of [l-l^cj-chlorododecanes in rela- tion to degradation and excretion in mice. Arch. Toxicol. 50(2).:217-226. Darnerud, P. O. and I. Brandt. 1982. Studies on the distribution and metabolism of a 14c-labelled chlorinated alkane in mice. Environ. Poll. (Ser. A) 27(l):45-56. Geyer, H., P. Sheehan, D. Kotzias, D. Freitag, and F. Korte. 1982. Prediction of ecotoxicological behaviour of chemicals: Relationship between physico- chemical properties and bioaccumulation of organic chemicals in the mussel Mytilus edulis. Chemosphere 11(11):1121-1134. Howard, P. H., J. Santodonato, and J. Saxena. 1975. Investigation-of selected potential environmental contaminants: Chlorinated paraffins. Final Report. Contract No. 68-01-3101.' Project L1259-05. U.S. EPA, Document EPA-560/2-75-007. 109 p. Linden, E., B.-E. Bengtsson, O. Svanberg, and G. Sundstrom. 1979. The acute toxicity of 78 chemicals and pesticide formulations against two brackish water organisms, the bleak (Alburnus alburnus) and the harpacticoid Nitocra spinipes. Chemosphere 8(11/12):843-851. Lcmbardo, P., J. L. Dennison, and W. W. Johnson. 1975. Bioaccumulation of chlorinated paraffin residues in fish fed Chlorowax 500C. J. Assoc. Off. ------- Anal. Chem. 58(4):707-710. Madeley, J. R. and R. D. N. Birtley. 1980. Chlorinated paraffins and the environment. 2. Aquatic and avian toxicology. Environ. Sci..Technol. 14(10):1215-1221. - * Renberg, L., G. Sundstrom, and K. Sundh-Nygard. 1980. Partition coeffients of organic chemicals derived from reversed phase thin layer chromatography: Evaluation of methods and application on phosphate esters, polychlorinated paraffins and some PCB-substitutes. Chemosphere 9(11):683-691. Stetten, N. D., Jr. 1943. Metabolism of a paraffin. J. Biol. Chem. 147( ): 327-332. Svanberg, 0. 1978. Chlorinated paraffins — A case of accumulation and toxicity to fish. Ambio 7(2):64-65. Svanberg, O. and E. Linden. 1979. Chlorinated paraffins — An environmental hazard? Ambio 8(5):206-209. Tarkpea, M., E. Linden, B.-E. Bengtsson, A. Larson, and 0. Svanberg. 1981. Nat. Swed. Environ. Prot. Bd., Brackish Water Tox. Lab., Rep. NBL Rapp. 111. 22 p. Zitko, V. 1974. Uptake of chlorinated paraffins and PCB from suspended solids and food by juvenile Atlantic salmon. Bull. Environ. Contain. Toxicol. 12(4):406-412. ------- Table 1. Tiered testing scheme agreement published in the Federal Register on January 8, 1982 between the Chlorinated Paraffins Consortium and the Environmental Protection Agency. Phase I Testing * Percent Chlorination by Weight Carbon Chain Length: c 10-12 C 14-19 C 20-30 40 to 50 % Cl | 50 to 60 % Cl | 60 to 70 % Cl ** liquid - 58 % Cl liquid - 52 % Cl liquid - 43 % Cl solid - 70 % Cl ** Each compound was tested for 60-day lethal and sublethal effects on mussel (Mytilus edulis) and rainbow trout (SaLno gairdneri ) . According to chlorine content (58 percent), the short chain length paraffins belong in this column and not the column indicated in the Federal Register. Phase II Testing Additional testing was to be conducted on the 58 % chlorinated short chain (^10-12) length paraffins, which were already known to be the most toxic from Phase I. The tests included: Growth (rainbow trout and mussel) Bioconcentration (rainbow trout and mussel)-v Life Cycle (Daphnia) - Life Cycle (mysid shrimp)- ^> Embryo-juvenile (sheepshead minnow) 14-Day Bioassay (freshwater alga) 14-Day Bioassay (marine alga) Chronic (partial life-cycle) (midge) w^'* Solubility Biodegradation (aerobic and anaerobic) Avian Study (test substance to be selected)*** Reproductive Study (duck)**** Received and Validated X X X X X X X X X X X X X X X X X not validated X not validated X X X . X *** Remarks made by the Chlorinated Paraffins Corsortium indicate that this study refers to the duck reproduction study and is not a separate study. **** This study is not a part of the proposal by the International Chlorinated Paraffins Manufacturers Consortium, but it was submitted by the American members of the Consortium. ------- Table 2. Results of Phase I and Phase II testing on rainbow trout and mussels. Rainbow Trout Salmo gairdneri 60-Day LC50 Abnormal Growth Whole Animal Behavior MATC BCF Overall MATC Short-chain (Cio-12) 58 % Cl Intermediate-chain 52 % Cl Long-chain (C20-30> 43 % Cl 70 % Cl 200 ug/1 < 33 ug/1 (340 ug/D* (continuing deaths) (33 ug/1 - 33% dead) > 3.4 - < 17.2 ug/1 (26% increase in weight growth rate) > 4,500 ug/1 (3 % dead; no control deaths) » 4,000 ug/1 (0 deaths) > 3,800 ug/1 (3 % dead; 3-6% control deaths) > 1,050 - < 4,500 ug/1 (transient on Days 5, 8, & 9) > 4,000 ug/1 (all normal) abnormal behavior in all groups (highest effect in controls) 3550-5260 > 3.4 < 17.2 ug/1 (increased weight) 45 - 67** 1,050 < 4,500 ug/1 (abnormal behavior) 18 - 38** 6 - 54** > 4,000 ug/1 (no effect) > 3,800 ug/1 ' (no sign. effect)- * This reported value has been replaced by a lower estimated toxicity level. ** These bioconcentration factors are preliminary and have not been confirmed by acceptable studies. ------- Table 2. (Cont.) Short-chain (Cio-12) 58 % Cl Intermediate-chain 52 % Cl Long-chain (C20-30> 43 % Cl 70 % Cl Mussel Mytilus edulis 60-Day LC50 Abnormal Behavior Growth MATC Whole Animal BCF Overall MATC 74 ug/1 (68 - 81) (chronic mortality) » 3,800 ug/1 (2 % death at 220 ug/1; 0 - 4 % control deaths) » 2,180 ug/1 (0 deaths) »1,330 ug/1 (0 deaths) < 13 ug/1 (occasional reduction in feeding) > 2.3 - < 9.3 ug/1 (53 % red. in tissue and shell growth rates) 24,800-40,900 > 2.3 < 9.3 ug/1 (growth reduction) < 220 ug/1 (transient reduction in feeding) < 3,800 ug/1 (consistent red. in feeding) > 120 - < 2180 ug/1 (consistent reduction in feeding) > 460 - < 1330 ug/1 (marginally reduced feeding) 430- 2,860* < 220 ug/1 (abnormal behavior) 260- 1,160* > 120 < 2,180 ug/1 (abnormal behavior) 220- 340* > 460 < 1,330 ug/1 (abnormal behavior) These bioconcentration factors are preliminary and have not been confirmed by acceptable studies. ------- Table 3. Acute toxicity values for Chlorowax reported by Johnson and Finley (1980). 96-Hour LC50 (ng/1) Bluegill Channel Fathead Rainbow Sunfish Catfish Minnow Trout Chlorinated Carbon % Paraffin Length Cl Chlorowax 500C 10-13 59 > 300 Chlorowax 40 20-30 40 > 300 Chlorowax LV 20-30 46 > 300 Chlorowax 50 20-30 50 > 300 Chlorowax 70 20-30 70 > 300 > 300 > 100 > 300 > 300 > 300 > 300 > 300 "Note: Variations in test temperature between 5° and 25°C did not reduce the static toxicity of Chlorowax 500C below a 96-h LC50 value of 300 mg/1. Sublethal effects were noted in flow-througfh tests with rainbow trout in concentrations as low as 40 ug/1." Table 4. Acute toxicity values for bleaks exposed to chlorinated paraffins (Linden et al., 1979). Chlorinated Paraffin Witaclor 49 Witaclor 55EN Witaclor 63 Witaclor 71P Chlorparaffin huls 70C Chlorparaff in huls 40G Witaclor 50 Cereclor S52 Cereclor 42 Carbon Length 10-13 10-13 10-13 10-13 11.5 15.5 14-17 14-17 22-26 % Cl 49 56 63 56 70 40 50 52 42 96-Hour LC50 (ng/1) Bleaks (Alburnus alburnus) > 5,000 > 10,000 > 5,000 > 5,000 > 10,000 > 5,000 > 5,000 > 10,000 > 5,000 ------- Table 5. Acute mammalian toxicity values summarized by Howard et'al_. (1975) for various chlorinated paraffins. Acute Oral LD50 (g/kg) Chlorinated Paraffin Chlorowax 500C Chlorowax 40 Chlorowax 70 Chlorez 700 Khp 470 Carbon Length 10-13 20-30 20-30 20-30 % Cl 59 40 70 70 48 Rat > 21.5 » 10 » 50 » 50 26.1 Mouse Guinea Pig » 25 » 25 21.85 » Indicates no mortality at or below that dose level. Table 6. Acute toxicity values reported by Madeley and Birtley (1980) for two chlorinated paraffins. Acute Oral Subacute Dietary 96-Hour LD50 (gAg) LC50 (ppm) LC50 (ug/1) Ring-necked Mallard Ring-necked Mallard Rainbow Pheasant Duck Pheasant Duck Trout Chlorinated Carbon % Paraffin Length Cl Cereclor S52 14-17 52 » 24.606 » 10.280 » 24,063 » 24,063 (loss of (reduced^ weight) feeding) Cereclor 42 20-30 42 » 770* » Indicates no mortality at or below that dose level. * Toxicity value too high (water solubility was exceeded as indicated by the reported presence of an opaque emulsion). ------- Table 7. Growth effects on weight and length caused by 58% chlorinated short (CIQ-IS) chain length n-paraffins in rainbow trout and sheepshead minnow. Percent Difference Compared to Solvent Controls Weight Length Test Concentrat ion (ug/1) 2.4 3.4 4.1 6.4 17.2 22.1 33 36.2 54.8 71.0 100 161.8 279.7 350 620.5 1,070 3,050 Rainbow Sheepshead Trout Minnow + 3.8 + 0.02 + 14.9* + 31.3* + 25.4* + 27.5* + 37.9** + 21.3* + 31.7* + 15.1* + 13.5** + 13.0 + 1.9 - 3.1** - 30.9* - 57.6** - 74.7** Rainbow Sheepshead Trout Minnow + 4.0* + 0.7 + 3.7* + 5.5* + 6.2 + 7.2* + 34.2** + 7.4* + 6.4* + 5.6* + 6.7** + 3.4* + 1.9 - 1.9** - 9.2* - 28.7** - 32.6** * Statistically significant (P £ 0.05) differences conpared to the acetone control. ** Statistical analyses were not reported for these values. ' ------- Table 8. Time to lethality (LT50) in juvenile Atlantic saliton (zitko, 1974). Control Cereclor 42 Chlorez 700 Carbon Length % Cl 20-30 42 20-30 70 Feeding Cone. (ug/g) 10 100 10 100 LT50 (days) 138 47 80 71 39 ------- Table 9. Bioconcentration studies and BCF values resulting from the uptake of residues from the water column as reported in Consortium generated studies and in published literature. Chlorinated Paraffin Carbon (Data Source) Length Short Chain 10-13 (Consortium, unpublished) Short Chain 10-13 - Intermediate Chain 14-17 Long Chain 20-30 Long Chain 20-30 Short Chain 10-13 (Consortium, unpublished) Short Chain 10-13 Intermediate Chain 14-17 Long Chain 20-30 Long Chain 20-30 Exposure % Test Species Time Route Cl (days) 59 Mussels 59 Mussels 52 Mussels 43 Mussels 70 Mussels 59 Rainbow Trout 59 Rainbow Trout 52 Rainbow Trout 43 Rainbow Trout 70 Rainbow Trout 147 91 60 60 60 60 60 60 60 60 60 60 168 168 60 60 60 60 60 60 60 60 60 60 60 60 Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water BCF Cone, (whole (ug/1) animal) 2.35 10.1 13 44 71 130 220 3,800 120 2,180 460 1,330 3.1 14.3 33 100 350 1,070 3,050 1,050 4,500 s 970 4,000 840 1,900 3,800 40,900 24,800 329 723 411 12,177 2,856 429 1,158 261 341 _ 223 3,550 5,260 7,155 7,816 3,723 2,642 1,173 44.9 66.7 17.9 37.6 53.8 5.7 32.5 7 7 ------- Table 9. (cont.) Chlorinated Paraffin Carbon (Data Source) Length Huls chlorparaff in 10-13 70C (Svanberg et al.r 1978) Witaclor 149 10-13 (Bengtsson et - al., 1979) Witaclor 159 10-13 Witaclor 171P 10-13 Witaclor 350 14-17 Witaclor 549 18-26 PCB (Clophen A50) Cereclor 42 20-30 (Zitko, 1974) Chlorez 700 20-30 PCB (Aroclor 1254) % Cl 70 49 59 70 50 49 50 42 70 54 Test Species Bleaks Bleaks Bleaks Bleaks Bleaks Bleaks Bleaks Atlantic salmon Atlantic salmon Atlantic salmon Exposure Time Route (days) 15 28 29 27 29 14 14 14 14 14 14 2 6 2 6 1 2 6 Water Water Water Water Water Water Water Water Water Water Water Suspended solids Suspended solids Suspended solids Water BCF " Cone, (whole (ug/1) animal) 0.1 0.1 0.1 1.0 1.0 125 125 125 125 125 125 ib lb Ib 2033 328* 262 47.5a 28.6 760 720 160 40 20 1920 0.44C 0.75C 0.22C 0.46C 19. 9C 28. 3^ 134C a These Bcf values were derived from single fish that died during- the study. b since the concentration of suspended solids in the water was not reported, the value indicated is the concentration of chlorinated paraffins that was adsorbed onto suspended solids in the water column. c These BCF values are reported as chlorine (ug/g wet wt.) in fish, because the final concentration of test material present in the water column is unreported. ------- Table 10. Bioconcentration studies and BCF values reported in the literature for the uptake of chlorinated paraffin residues in food. Chlorinated Paraffin Carbon (Data Source) Length Chlorowax 500C 10-13 (Lombardo et al., 1975) Witaclor 149 10-13 (Bengtsson and Ofstad, 1982) Witaclor 149 10-13 Witaclor 149 10-13 Witaclor 171P 10-13 Witaclor 549 18-26 Cereclor 42 20-30 (Zitko, 1974) Chlorez 700 20-30 PCB Aroclor 1254 Test % Species Cl 60 Rainbow trout 49 Bleaks 49 Bleaks 49 Bleaks 71 Bleaks 49 Bleaks 42 Atlantic salmon 70 Atlantic salmon 54 Atlantic salmon Exposure Time Route (days) 82 91 91 91 91 91 33 109 181 33 109 181 33 109 181 33 109 181 33 109 181 33 109 181 Food Food Food Food Food Food Food Food Food Food Food Food Cone. (ug CP/ g food) 10 590 2500 5800 3180 3400 10 100 10 100 10 100 '^ BCF Uptake Efficiem 2.759 3 41a 45 9a 10 4.6a 5 5.53 6 2a 2 O.llb nd nd O.Slb nd nd 0.29b nd nd 0.49b nd nd 3.86b 3.80b 3T.88b 13. 9b 24. Ob 30. Ob a These BCF values were calculated as using the total daily consumption level of chlorinated paraffins as the exposure level. t> These values are reported as chlorine (ug/g wet wt.) in fish, because BCF values could not be calculated without knowing the amount of toxicant eaten. ------- Table 11. Characteristics indicative of bioconcentration potential in fish for various groupings of chlorinated paraffins. Chain Length ClO-13 H20 Sol.(ug/l) log P BCF fron: H20 - max. (60 days) (14 days) Food - max. (91 days) Rates of: Accumulation Depuration C14-17 H20 Sol.(ug/l) log P BCF from: H2O - max. (60 days) (14 days) Food Rates of: Accumulation Depuration C18-26 H20 Sol.(ug/l) log P BCF from: H2O - max. (14 days) Food (91 days) Rates of: Accumulation Depuration C20-30 H20 Sol.(ug/l) log P BCF fron: H20 - max. (60 days) Food Rates of: Accumulation Depuration Percent Chlorination 42 - 50 59 - 60 -70 - 71 4.39 - 6.93 760 ( 125 ppb) 33 ( 590 ppm) 10 (2500 ppm) 95 - 470 (Cjj) 4.48 - 7.38 3,550 - 5,260 1,173 - 7,816 720 ( 125 ppb) fast and constant fast and constant 92% loss in 7 days half-lives of 9 to 21 days 5-27 (C15) 5.47 - 8.21 64 ( 125 ppb) slow little in 7 days 7.46 - 12.83 32 ( 125 ppb) 2 (3400 ppm) slow and constant less than 50% loss in 316 days 3.6 - 6.6 (C25) 8.69 ->12.83 17.9 - 37.6 44.9 - 66.7 5.37 - 8.69 160 ( 125 ppb) 6 (3180 ppm) fast and constant less than 50% loss in 316 days 6 (C25) '5.7'- 32.5 ------- Figure 1. EC50 chronicity in the waterflea Daphnia magna following exposure to 58 % chlorinated short chain (Cio_i3) length n-paraffins. 600 500 C o n c e n 400 t r a t o n 300 i n g / 200 1 100 456 Time (days) 10 * The acute 48-hour EC50 value reported in the daphnid study. ------- Figure 2. Growth effects on weight caused by 58% chlorinated short chain length n-paraffins in rainbow trout and sheepshead minnows. P e r c e n t o f 50 40 30 20 10 S o i q V e n -10 t X 0 0 « o x o c o h t r o 1 G r o w t h -20 -30 -40 -50 -60 -70 • -80 X \ I T 10 100 1,000 log Test Concentration (ug/1) 10,000 (X) - Rainbow Trout (0) - Sheepshead Minnow ------- Figure 3. Growth of the marine alga, Skeletonema costatum, cultured in a 58 % chlorinated short chain (^0-13) length n-paraffin (particle count). CO LU -J CJ cc 0= Q. 10 DflYS ------- Figure 4. Growth of the freshwater green alga, Selenastrum capricornutum, cultured in 58 % chlorinated short chain (Cio_i3) length n-paraffin (particle count). cn LJ u CE L9 KEY f O QJNTHUL ——SOL. CONTRJL O % 0.18 MCA. * B.32 HC/, t 1.55 MCA. l.J MC/L 1.8 MC/L —X- 3.2 MCA. DflYS ------- APPENDIX. Results of Phase II testing of 58 % Chlorinated Short-Chain Length (Cio-12) n-Paraffins on additional species. Test Species Test Type LC50 Overall MATC MATC MATC Hatchability Survival (percent) (percent) MATC % Growth Rate Length Weight Sheepshead Minnow Embryo-larvae Cyprinodon variegatus (Study # 1) (Study I 2) > 2.4 < 4.1-55 ug/1 (increased growth) > 55 ug/1 > 55 ug/1 > 2.4 - > 2.4 (77-95) (68-90, 55 ug/1 <4.1-55 ug/1 88 -100) (4 - 7 % (14 - 31 % increase) increase) < 36-71 < 162 ug/1 > 620 ug/1 > 620 ug/1 < 36- 71 (increased growth) (80 - > 280 < 620 ug/1 (reduced growth) 95) (65.8- 90.7, < 162 ug/1 75.8-100) (5 - 7 % increase) > 280 - < 620 ug/1 (9 % red.) Waterflea Daphnia magna Life-cycle Mysid Shrimp Life-cycle Mysidopsis bahia 530 ug/1* 46 ppb (48-hr EC50) 12 ug/1* 8.9 < 16.3 ug/1 (6-21 day EC50) 14.1 ug/1* < 14.1 ug/1 (96-hr LC50) < 2.7 ug/1* < 2.7 ug/1* (reduced young (44 % red. per female) offspring < 8.9 ug/1* /female) (66 % red. in total reprod.) > 7.3 < 13.7 ug/1* > 5.0 - > 0.6 < 1.2 ug/1 < 7.3 ug/1 (sign, parental (33 % red. mortality) offspring /female) Midge Life-cycle Chironomus tentans > 162 ug/1 (48-hr LC50 no deaths) > 60 < 78 ug/1 (red. hatching) > 60 - < 78 ug/1 (60 % red. hatching) < 36- 71 < 162 ug/1 (15 - 21 % increase) > 280 - < 620 ug/1 (31% red.) > 5.0 - > 8.9 ug/1* < 8.9 ug/1* (1 % red.) (37 % dead offspring not sign.) > 0.6 - > 7.3 ug/1 > 7.3 ug/1 < 1.2 ug/1 ( 1 % ( 0.4 % (40-50 % Increase) reduction) parental deaths) > 78 - < 78 ug/1 < 78 ug/1 < 121 ug/1 (10 % (1 % (no red. in red. in emergence) eggs/mass) hatch) Data value can not be used with confidence. ------- APPENDIX (Cont.) Test Species Test Type LC50 MATC Cell Growth (particle count) Green Alga Selenastrum capricomatum Acute 3,690 ug/1* > 1,200 ug/1 (96-hr EC50) 1,310 ug/1* > 1,200 ug/1 (10-day EC50) > 390 < 570 ug/1 (35 % reduction in growth) > 390 < 570 ug/1 (35 % reduction in cell growth) Marine Alga Skeletoneroa costatum Acute 31.6 ug/1 (48-hr EC50) 42.3 ug/1 (96-hr EC50) > 69.8 ug/1 (10-day EC50) > 12.1 < 19.6 ug/1 (44 % reduction in growth on Day 2) > 19.6 < 43.1 ug/1 (Day 4 - 34 % red.) > 69.8 ug/1 (Day 10 - no sign.) > 12.1 < 19.6 ug/1 (44 % reduction in growth on Day 2) > 19.6 < 43.1 ug/1 (Day 4 - 34 % red.) > 69.8 ug/1 (Day 10 - no sign.) * Data can not be used with confidence. ------- |