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HomeMy WebLinkAboutNC0083321_Report_20220908 SHEALY a TOXICITY IDENTIFICATION =+Y J"`" "•T _ EVALUATION • ONSLOW WATER AND SEWER AUTHORITY - HUBERT WATER TREATMENT PLANT 31144. - JUNE 2022 FINAL REPORT 4 1 s i • _r '� ' `� SUBMITTED BY: .‘ SHEALY CONSULTING, LLC Shealy Consulting , LLC ♦ 343 W. Columbia Avenue • Batesburg - Leesville, SC 29006 TOXICITY IDENTIFICATION EVALUATION FOR THE ONSLOW WATER AND SEWER AUTHORITY HUBERT WATER TREATMENT PLANT JUNE 2022 FINAL REPORT SUBMITTED BY: SHEALY CONSULTING, LLC BATESBURG-LEESVILLE, SOUTH CAROLINA Reported by: /L-t-►- ac-DA,,,' „, Laura Shealy Davis, President I SHEALY J TABLE OF CONTENTS SECTION PAGE NO. 1.0 EXECUTIVE SUMMARY 1 2.0 INTRODUCTION 2.1 Background 6 2.2 Site Visit and Toxicity Identification Evaluation Resumed 6 2.3 Scope of Work and Timeline 7 3.0 MATERIALS AND METHODS 3.1 Historical and Current Data Review 9 3.1.a Review of Previous Effluent Analytical Data 9 3.1.b Comparative Review of Hubert and Dixon Analytical Data 9 3.1.c Review of process Flows 9 3.1.d Review of Hubert WTP Source Water 9 3.1.e Review of Chemicals Used at the Hubert WTP 10 3.2 Sample Collection, Handling and Preservation 10 3.3 Toxicity Testing 10 3.4 Toxicity Persistence Testing 11 3.5 Identification of Lagoon Algae 11 3.6 Analytical Testing and Data Analyses 11 3.7 Phase I Toxicity Characterization Procedures 12 4.0 RESULTS AND DISCUSSION 4..1 Historical and Current Data Review 16 4.1.a Review of Previous Effluent Analytical Data 16 4.1.b Comparative Review of Hubert and Dixon Analytical Data 16 4.1.c Review of process Flows 17 4.1.d Review of Hubert WTP Source Water 20 4.1.e Review of Chemicals Used at the Hubert WTP 20 4.2 Toxicity Testing 22 4.3 Toxicity Persistence Testing 22 4.4 Identification of Lagoon Algae 23 4.5 Analytical Testing and Data Analyses 23 4.6 Phase I Toxicity Characterization Procedures 28 5.0 CONCLUSIONS 32 REFERENCES APPENDICES TOXICITY IDENTIFICATION EVALUATION FOR THE ONSLOW WATER AND SEWER AUTHORITY HUBERT WATER TREATMENT PLANT JUNE 2022 REPORT SECTION 1.0 EXECUTIVE SUMMARY The Onslow Water and Sewer Authority(ONWASA) of North Carolina operates the Hubert Water Treatment Plant (WTP) which discharges wastewater into Queen Creek (permit #NC0083321). The facility is required to conduct quarterly Whole Effluent Toxicity (WET) toxicity tests with the species Americamysis bahia at a test concentration of 90%. The facility experienced several failures of quarterly tests conducted prior to March 2020. The engineering firm of W.K. Dickson & Co, Inc. (WKD) requested that Shealy Consulting, LLC (Shealy), conduct a Toxicity Identification Evaluation (TIE) in response to these toxicity test failures. A toxicity identification evaluation (TIE) was performed June 2020 to November 2020, however after the study began, no further failures were observed for six(6) months and the study was terminated. Results from the TIE performed during 2020 were inconclusive and reported in a final report issued November 2020. In November 2021, WK Dickson & Co, Inc. (WKD) notified Shealy Consulting, LLC that the facility had experienced toxicity test failures for the September 2021 (37.5% mortality) and October 2021 (100% mortality). In November 2021, an additional failure was observed with 62.5% mortality followed by a passing toxicity test for December 2021. At this point, Shealy was asked to resume the TIE. The TIE was completed late May 2022 and the following conclusions were made as a result of the study: HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 1 SHEALY-. V As a part of the TIE process, past effluent analytical data (January—June 2020) for the Hubert WTP had been previously provided to Shealy for review. The analytical data from 2020 represented samples collected during a period in which toxicity passes and failures had been observed. It was previously determined that no obvious candidates for toxicity were identified with the available data and this opinion remained during this project. V The Dixon WTP which has a similar process as the Hubert WTP but also has RO treatment, consistently meets toxicity limits. As a result, analytical data from one sample collected February 2022 from the Dixon WTP was compared to data from the Hubert WTP collected the same day. The data from this testing indicated that the Hubert WTP effluent contained significantly higher concentrations of bromide, calcium, chloride, iron, magnesium, manganese, sodium, and sulfate than the Dixon WTP effluent. V The Hubert WTP process discharge volumes, specifically total, regeneration and backwash flows for February 1—April 21, 2022, were evaluated and compared to toxicity results during the study period. It was discussed at a January 2022 site visit that no obvious differences were apparent to ONWASA staff between the current flows from the various processes compared to 2020 and 2021 when the facility was passing toxicity. Nevertheless, daily flows from almost three (3) months were reviewed by Shealy personnel to determine variability. The Hubert WTP lagoon system is comprised of three (3) 750,000-gallon lagoons for a total of 2,250,000 gallons of water retention. Solids from Lagoon 1 have been dredged in the last several years, but dredging has not been accomplished in lagoons 2 and 3 and both have significant solids build up. Reviewing the data from February, March and April 2022 indicated significant variability in the total, regeneration, and backwash flows on a daily and weekly basis.This does not take into consideration rainfall during those months which would add additional volume to the lagoons increasing dilution but decreasing treatment retention. Since all toxicity SHEALY o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION results during February, March and April 2022 resulted in failures with similar mortality rates, there does not appear to be a significant link between flow rates and the toxicity observed. However, since it was established clearly in the previous TIE report (November 2020 TIE Report) that the Regeneration Process is by far the most toxic at the facility, it is reasonable to assume that flow rates from other processes and high rainfall could have some positive effect on toxicity simply by dilution. ✓ Solids build up in the lagoon system do not appear to be related to toxicity at the time of this study other than reducing retention time in the treatment lagoons. However, compounds generated in low dissolved oxygen environments such as those that most certainly exist in the Hubert WTP lagoons with solids build up, could have a negative impact on future results. Dredging the solids from all the lagoons on a regular basis would also be beneficial in extending the retention time through the system. ✓ Two (2) samples of source water were collected December 20 and December 21, 2021, from the red and blue raw water taps and the individual wells on each line. No constituents measured were suspected of beingat levels or close to levels that could be p contributing to toxicity. ✓ Two (2) chemicals used at the Hubert WTP were reviewed for the potential to cause toxicity, potassium permanganate and the stain removal product. It was determined with the use of Safety Data Sheets (SDS) for the products and additional research that neither of these products should be contributing to toxicity. ✓ A sample collected February 7, 2022, was initially tested for toxicity, and found to be acutely toxic (70% mortality). To determine the degree of toxicity persistence the sample was held for eleven (11) days and retested for toxicity. After that time period the sample remained similarly toxic (65% mortality). The fact that toxicity was persistent was one of the reasons that ionic imbalances or high ions was suspected as potentially playing a part in toxicity since this condition would be persistent over time. SHEALY v HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 3 ✓ There was a concern for toxic by-products by the algae build-up in Lagoons 2 and 3 at the Hubert WTP. As a result, a sample was collected May 2, 2022, and sent to the Clemson University Plant and Pest Diagnostic Clinic. Results from those analyses indicated that there were several species of green algae present, none of which would have toxic by-products. ✓ A total of eight (8) samples were collected for analytical testing between March 8 and April 26, 2022. For many of the analytes, including cations and anions, samples were tested with and without salt adjustment to 25 ppt, the toxicity test salinity. Most of the metals and all heavy metals that typically cause toxicity in effluents (Copper, Zinc, Nickel, Cadmium)were at concentrations well below toxic thresholds. Nitrogen compounds including ammonia, nitrate and nitrite were also all below detection limits. V From the beginning of the study there was a concern that ionic imbalances may be contributing to toxicity. The breakdown of major ion components in the Hubert WTP effluent after salt adjustment to 25 ppt (the toxicity test salinity)was compared to major ions in typical seawater at 25 ppt. Ions present in Hubert effluent samples at comparable levels to 25 ppt saltwater were bromide, chloride, sulfate, potassium, sodium, and strontium. Fluoride and calcium were consistently observed in the samples higher than seawater. ✓ The high end of the fluoride range (2.94 mg/I) observed in effluents was significantly higher than the average for seawater at 25 ppt. Fluoride is not toxic to Mysid Shrimp at this level based on previous Shealy lab experiments. In addition, Hubert effluent samples collected during the study period that contained little or no fluoride were also found to be toxic. ✓ Ions were measured for two (2) toxic samples and the ion imbalances calculated. It was believed that the relatively low concentrations of sodium (compared to seawater at comparable salinity) was likely the culprit for excess negative charge in the effluent. SHEALY HUBER T WTP "TOXICITY IDENTIFICATION EVALUATION 4 Because the imbalances calculated were about half the threshold for toxicity reported in the literature, it was not thought that ionic imbalance was the culprit for toxicity, although it is believed that it might be contributing. ✓ Calcium concentrations in Hubert WTP effluent were consistently three (3) to four(4) times higher than seawater at the same salinity. Unfortunately, there is no calcium data for samples collected during 2020 and 2021 that were passing toxicity. Concentrations observed for this study ranged from 646 mg/I —976 mg/I in the effluent without salt addition and 993 mg/I —1260 mg/I in effluent with salt adjusted to 25 ppt for testing. Typical seawater at 25 ppt contains approximately 300 mg/I of calcium. ✓ A literature search indicated that excess calcium has been found to be toxic to Mysid Shrimp at the levels observed in Hubert effluent and lower. The upper limit for the toxic threshold (no observed effect concentration, NOEC for acute toxicity) for calcium at 25 ppt for Mysid Shrimp has been reported as being approximately 600 mg/I. It is believed that high calcium concentrations were contributing to toxicity in the Hubert WTP effluent and was the major contributor during the study. ✓ Phase I toxicity characterization testing performed on a sample collected April 4-5, 2022, confirmed the conclusion that calcium was a major contributor of toxicity during the study. For this sample EDTA which forms a complex with calcium, reduced toxicity from 70% in the untreated sample to 15%which is significant. The calcium concentration of this sample was 993 mg/I, above the reported toxic threshold. SHEALY o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 5 SECTION 2.0 INTRODUCTION 2.1 Background The Onslow Water and Sewer Authority (ONWASA) of North Carolina operates the Hubert Water Treatment Plant (WTP) which discharges wastewater into Queen Creek (permit #NC0083321). The facility is required to conduct quarterly Whole Effluent Toxicity (WET) toxicitytests with the species Americamysis bahia at a test concentration of 90%. The facility p Y experienced several failures of quarterly tests conducted prior to March 2020. The engineering firm of W.K. Dickson & Co, Inc. (WKD) requested that Shealy Consulting, LLC (Shealy), conduct a Toxicity Identification Evaluation (TIE) in response to these toxicity test failures. A toxicity identification evaluation (TIE) was performed June 2020 to November 2020, however after the study began, no further failures were observed for six (6) months and the study was terminated. Results from the TIE performed during 2020 were inconclusive and reported in a final report issued November 2020. In November 2021, WK Dickson & Co, Inc. (WKD) notified Shealy Consulting, LLC that the facility had experienced toxicity test failures for the September 2021 (37.5% mortality) and October 2021 (100% mortality). In November 2021, an additional failure was observed with 62.5% mortality followed by a passing toxicity test for December 2021. 2.2 Site Visit and Toxicity Identification Evaluation Resumed On January 20, 2022, personnel from ONWASA, WKD and Shealy met at the Hubert WTP to tour the facility and discuss the project. During that site visit, a thorough discussion was held of any changes made to processes, chemicals used in the various processes or changes to the lagoon system that might contribute to the recent toxicity. It was not understood why the Hubert WTP had only passing toxicity tests from June 2020 until September 2021. With no likely candidates for toxicity identified at that time, the TIE was re-implemented for the facility. The wastewater treatment facility consists of three (3) lagoons and one (1) overflow lagoon. Wastewater from the WTP includes backwash from greensand and carbon filtration in addition SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION �� to reject wastewater from ion exchange units. A more detailed discussion of the treatment system with diagram can be found in the November 2020 Final TIE Report. During a site visit in January 2022, it was observed that the second and third lagoons contained a high degree of algae. A contributing factor to the algae was Canadian Geese, dozens of which were present at the time of the visit. It was further observed that the lagoon area contained a very high concentration of Canadian Geese droppings which likely caused nutrient loading to the lagoon system. As a result, it was determined that nutrients in the Hubert WTP effluent would be analyzed along with the identification of the algae. 2.3 Scope of Work and Timeline A tentative scope of work was developed with the understanding that modifications might need to be made as the study progressed and submitted February 3, 2022, to WKD and ONWASA. The TIE would include four(4) separate tasks. Task 1 was completed during the 2020 TIE work and involved an initial meeting and tour of the WTP, and review of all available analytical data. All the previous data generated would be reviewed again during this task. Tasks 2, 3 and 4 would be performed concurrently.Task 2 would involve collecting analytical data on primarily effluent (and possibly process area and combined influents) over some time period. Identification of the lagoon algae would be performed during this task. This task was expanded to include an examination of all major ions present in the effluent in the event that ionic imbalance was the cause of effluent toxicity for the Hubert WTP. Task 3 would be to perform toxicity identification (Phase I) characterization procedures on at least two (2) samples found to be significantly toxic to determine the group of toxicants that may be involved in toxicity. Task 4 was to develop a quality control checklist to be used by the NPDES laboratory each time a routine toxicity test is performed. An approximate timeline of activities for the project is provided in Figure 1. SHEALY H, (si is �� ��_�t l 1 i!)I v 01, `,I 7 FIGURE 1: TIMELINE FOR TIE ACTIVITIES May 24,2022, Review of Historical Analytical Memo prepared and source Water Analytical summarizing Data Analytical Data Gathered Weekly findings JAN. 2022 FEB. 2022 MARCH 2022 APRIL 2022 MAY 2022 JUNE 2022 Initial Site Visit Toxicological Phase I Review of all data, and Preparation of Review of Toxicity research and Final Report Scope of Work Chemicals Used Characterization conclusions and QC at WTP Testing Checklist Prepared and submitted SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION S SECTION 3.0 MATERIALS AND METHODS 3.1 Historical and Current Data Review 3.1.a Review of Previous Effluent Analytical Data As a part of the TIE process, past effluent analytical data (January—June 2020) for the Hubert WTP had been previously provided to Shealy for review. This data was reviewed for a second time. The data reviewed included the following: ✓ Total dissolved Solids (TDS) V Total Phosphorus ✓ Turbidity V Copper ✓ Total Suspended Solids (TSS) V Iron ✓ Salinity V Manganese ✓ Specific Conductance V Zinc V Total Nitrogen V pH ✓ Chlorde 3.1.b. Comparative Review of Hubert and Dixon Analytical data The Dixon WTP which has a similar process as the Hubert WTP but also has RO treatment, consistently meets toxicity limits. As a result, analytical data from one sample collected February 2022 from the Dixon WTP was compared to data from the Hubert WTP collected the same day. 3.1.c Review of Process Flows The Hubert WTP process discharge volumes, specifically the total, regeneration and backwash process volumes for February 1—April 21, 2022, were evaluated to determine variability and compared to toxicity results. 3.1.d Review of Hubert WTP Source Water Two (2) samples of source water were collected December 20 and December 21, 2021, from the raw water red and blue taps and individual wells on each line. From the red source water tap, samples from wells#1, #2, #4, #7, #11 and#14 were analyzed. From the blue source water SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 9 tap, samples from wells#3, #6, #8, #9,#10, #12, #13 and #15 were analyzed. The following parameters were measured for each sample: ✓ Nitrate ✓ Calcium ✓ Sodium ✓ Nitrite ✓ Potassium ✓ Silica ✓ Bromide ✓ Iron ✓ Magnesium ✓ Chloride ✓ Manganese ✓ Total hardness ✓ Fluoride ✓ Conductivity ✓ Phosphate-P ✓ Sulfate V Alkalinity ✓ Ortho-phosphate 3.1.e Review of Chemicals Used at the Hubert WTP Two (2) chemicals used at the Hubert WTP were reviewed for the potential to cause toxicity, potassium permanganate and the stain removal product. Specific details evaluated included usage rates at the WTP, aquatic toxicity, solubility, biodegradability, fate, and persistence. 3.2 Sample Collection, Handling and Preservation Effluent samples were collected for toxicity, phase I and analytical testing throughout the course of the study by Hubert WTP personnel and were transported to the various testing laboratories. Shealy Consulting, LLC were responsible for transporting samples collected for the two (2) phase I characterization test series. Water samples were collected as composites. All samples were transported on ice and were maintained in refrigerator units until used in testing. 3.3 Toxicity Testing Toxicity testing using the NPDES test species Amercamysis bahia (Mysid Shrimp) was conducted throughout the course of this project and all tests resulted in failures. Toxicity samples were collected twice during the months of March and April 2022 to obtain toxic samples on which to perform Phase I characterization testing. All routine NPDES testing toxicity testing was performed by Environmental Testing Solutions, Inc.,Asheville, North Carolina. SHEALY v HUBERT WTP TOXICITY IDENTIFICATION EVALUATI(>\ 10 3.4 Toxicity Persistence Testing The sample collected February 7, 2022, was initially tested, and found to be acutely toxic (70% mortality). To determine the degree of toxicity persistence the sample was held in cold storage for eleven (11) days and retested for toxicity. 3.5 Identification of Lagoon Algae During the site visit in January 2022, it was observed that the second and third lagoons contained a high concentration of algae. As a result, it was determined that the identification of the algae was necessary as certain types of algae release toxic metabolic products. A composite sample of lagoon algae was sent to the Clemson University Plant and Pest Diagnostic Laboratory for analyses. 3.6 Analytical Testing and Data Analyses As previous indicated, during the site visit, it was observed that the second and third lagoons contained a high concentration of algae. A contributing factor to the algae was Canadian Geese, dozens of which were present at the time of the visit. It was further observed that the lagoon area contained a very high concentration of Canadian Geese droppings which likely caused nutrient loading to the lagoon system. As a result, it was determined that nutrients in the Hubert WTP effluent would be analyzed. It was also determined during the initial site visit that more analytical data for the Hubert WTP effluent was necessary. The following analyses was performed on samples of Hubert WTP effluent collected weekly during March and April 2022 including various inorganics, ions, and metals.The ONWASA analytical laboratory performed all the analyses except metals. The metals analyses were conducted by Environmental Chemist, Inc., Wilmington, NC. The ion constituents were analyzed for both unadjusted and salt-adjusted effluent samples and imbalances quantified for each sample. Ionic imbalance is defined as a combination of salts in an effluent that (1) are present at levels or in ratios inconsistent with those normally found in SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 11 most naturally occurring waters; and (2) demonstrate toxicity during a WET test.These salts are normally referred to as total dissolved solids (TDS). High positive or negative imbalances,toxic levels of ions or the lack of necessary ions would all be candidates for toxicity. 3.7 Phase I Toxicity Characterization Procedures To characterize the toxicant(s) present in the Hubert WTP effluent samples, a battery of toxicity characterization tests was performed. These tests were performed in the BT Solutions, LLC laboratory located in Batesburg-Leesville, SC. These manipulations were not toxicant specific but intended to identify the group of toxicants responsible for toxicity. The TIE manipulations and subsequent toxicity test procedures were conducted in accordance with Methods for Aquatic Toxicity Identification Evaluations, Second Edition. (EPA/600/6-91/003).The Phase series was performed on two (2) samples previous found to be toxic. The tests were conducted by subjecting aliquots of the sample to specific treatments. The TIE manipulations were performed as soon as possible after original test results were known and samples retrieved from the Hubert WTP. The Hubert WTP had collected an extra three (3) gallons each time a toxicity sample was collected during the screening process and held in cold storage. Samples were manipulated and tested at 100%with no dilution. Salt water prepared for the laboratory controls and to adjust the effluent salinity was accomplished using Crystal Sea®Marinemix. This commercial sea salt does not contain EDTA and is the same sea salt used for Hubert WTP compliance toxicity testing. Salt water was prepared and allowed to aerate prior to use in testing.Testing was conducted in a room that provided isolation and the ability to regulate temperature.Temperature was monitored and remained between 24-26°C. Lights were set for a 16-hour light and 8-hour dark photoperiod. Light intensity was checked and confirmed to be between 50-100 foot-candles. The following procedures were used to prepare the Phase I test samples: SHEALY v I Il 13I IZ I \\ I I' I O\ICI H IDEA III IC y I Hy I.v vl I v I IOy 12 Untreated The purpose of the untreated test treatment was 1) to determine if the sample was still toxic after a time of refrigerated storage, and 2)to determine a baseline toxicity level upon which to compare the Phase I manipulated treatments. For this treatment, the effluent was stored in a sealed container in the refrigerator until used in testing. The sample was not manipulated in any way prior to testing other than salinity adjustment to 25 ppt. Aeration This test characterizes toxicants as volatile or oxidizable compounds.To conduct the aeration test, one aliquot of the Hubert WTP effluent was aerated at the initial pH for two (2) hours using diffused ambient air through a small pore stone. No foaming was noted during the aeration process in the sample. After treatment, the effluent was adjusted for salinity to 25 ppt. Aeration with pH 3 Adjustment The aeration test was also conducted with the pH of the sample reduced to 3 Standard Units (S.U.) There were concerns of the generation of sulfur compounds in the lagoon bottom sediments. The USEPA's aquatic life criterion for hydrogen sulfide is 2 ug/L(0.002 mg/L) for freshwater and saltwater species (USEPA, 1986). Sulfide exists as predominately two species in aqueous state, the bisulfite ion, and the more toxic hydrogen sulfide. The lower the pH of the solution, the more H2S and bisulfite gas that exits the solution. As a result, the pH3/aeration test is useful in determining if sulfur compounds are playing a role in toxicity. To conduct the test, one aliquot of the effluent was pH adjusted to 3.0 SU using hydrochloric acid and aerated for two (2) hours using diffused ambient air through a small pore stone. No foaming was noted during the aeration process in either sample. The post-aerated effluent originally adjusted to 3.0 SU was re-adjusted to a pH of about 7.5 standard units (SU) prior to toxicity testing. After treatment the effluent was adjusted for salinity to 25 ppt. SHEALY ;y , WO I ,\. . � �� 0 13 J Aeration with pH 11 Adjustment The aeration test was also conducted with the pH of the sample raised to 11 Standard Units (S.U.), aerated and re-adjusted to pH of about 7.5 SU prior to toxicity testing. After treatment, the effluent was adjusted for salinity to 25 ppt. Filtration The purpose of the filtration test was to determine if toxicant(s) could be removed by filtering the effluent through a glass fiber filter. This test characterizes toxicants as particulate material or associated with particulate matter. Using a vacuum pump, the sample was filtered through a clean glass fiber filter. After treatment, the Hubert WTP effluent was adjusted for salinity to 25 ppt. Filtration/pH3 To conduct the test, one aliquot of the effluent was pH adjusted to 3.0 SU using hydrochloric acid and filtered through a glass fiber filter.The post-filtered effluent originally adjusted to 3.0 SU was re-adjusted to a pH of about 7.5 SU prior to toxicity testing. After treatment, the effluent was adjusted for salinity to 25 ppt. Filtration/pH11 To conduct the test, one aliquot of the effluent was pH adjusted to 11 SU using sodium hydroxide and filtered through a glass fiber filter.The post-filtered effluent originally adjusted to 11 SU was re-adjusted to a pH of about 7.5 SU prior to toxicity testing. After treatment, the effluent was adjusted for salinity to 25 ppt. EDTA Chelation Ethylenediamenetetraacetic acid (EDTA) is a compound that chelates with metals and can Y p render some metals non-toxic to aquatic organisms. The purpose of this test was to determine if toxicity could be removed by adding EDTA to the effluent sample, which would indicate that the compound(s) causing toxicity were metals. Since the ability of EDTA to remove toxicity depends on the amount of metal present and other unknown variables, several different doses SHEALY o III Ni R 1 \\ i i 1 0\li_ 1 i t IU1 \1 11 IC \ 1 10\ i \ \I 1 \ 1 10\ 14 of EDTA were added to the effluent and tested. EDTA was added to aliquots of 100% Hubert WTP effluent to produce final concentrations of 19.0, 38.0, 75.0, 150 and 300 mg/L EDTA. The concentrations of EDTA used in the study bracketed the published LC50(concentration at which 50%or the organisms expire) for marine species.The EDTA-conditioned samples were allowed a contact time of at least two (2) hours prior to being subjected to toxicity testing. After treatment, the effluent was adjusted for salinity to 25 ppt. Carbon-18 Solid Phase Extraction at pH initial, pH3 and pH9 The purpose of the carbon-18 solid phase extraction test was to determine if toxicant(s) could be removed by passing the effluent through a carbon-18 solid phase extraction column. This test characterizes toxicants as being non-polar organic compounds. The effluent was filtered through a clean glass fiber filter. The filtrate was collected and then passed through a carbon- 18 solid phase extraction column. Aliquots of effluent were put through each of three C-18 columns at initial pH, pH of 3 and pH of 9. After treatment,the effluent was adjusted for salinity to 25 ppt. Oxidant Reduction Sodium thiosulfate is a compound that can reduce toxic compounds such as chlorine, iodine, and bromine to non-toxic forms. It also chelates with certain metals. The purpose of this test was to determine if toxicity could be reduced by adding sodium thiosulfate,thus indicating that the toxic component might be an oxidant. Sodium thiosulfate was added to aliquots of 100% Hubert WTP effluent to produce final concentrations of 6.3, 12.5, 25, 50 and 100 mg/L. The concentrations of sodium thiosulfate used in the study bracketed the published LC50 (concentration at which 50% or the organisms expire) for marine species. The conditioned samples were allowed a contact time of at least two (2) hours prior to being subjected to toxicity testing. After treatment, the effluent was adjusted for salinity to 25 ppt. SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 1 5 SECTION 4.0 RESULTS 4.1 Historical and Current Data Review 4.1.a Review of Previous Effluent Analytical Data As a part of the TIE process, past effluent analytical data (January—June 2020) for the Hubert WTP had been previously provided to Shealy for review. The analytical data from 2020 represented samples collected during a period in which toxicity passes and failures had been observed. The data was reviewed again for this project. During a January 2022 site visit, a discussion concerning any trends or changes to the routine and NPDES analytical data was held and indicated that no major changes in analytical results had occurred in late 2020 or 2021 when toxicity was consistently passing. Table 1 provides the ranges of analytical results from data collected January—June 2020. It was previously determined that no obvious candidates for toxicity were identified with the available data and this opinion remained during this project. As a result, it was determined that more analytical data was necessary and a schedule for weekly testing prepared. 4.1.b Comparative Review of Hubert and Dixon Analytical data The Dixon WTP which has a similar process as the Hubert WTP but also has RO treatment, consistently meets toxicity limits. As a result, analytical data from one sample collected February 2022 from the Dixon WTP was compared to data from the Hubert WTP collected the same day. Results from these tests are included in Appendix A.The data from this testing indicated that the Hubert WTP effluent contained significantly higher concentrations of bromide, calcium, chloride, iron, magnesium, manganese, sodium and sulfate than the Dixon WTP effluent. At the time of this review, it was not known if any of these constituents contributed to toxicity. SHEALY o III 13I_R 1 \\ II' 10)\1( 1 11 II)I y I lI I( \ I IUy i \ vI l v 11o\ 16 Table 1: Ranges of Analytical Results from Samples Collected from the Hubert WTP Effluent January—June 2021 Parameter Monitoring Period Range of Results Conductivity Monthly 7600—9530 umhos/cm Salinity Monthly 4.88—6.37 ppt pH Monthly 7.05-7.65 SU TSS Monthly <2.5—4.5 mg/I Chloride Monthly 2760—3450 mg/I TDS Monthly 5380—7720 mg/I Turbidity Monthly 0.73— 1.69 mg/I Total N Quarterly All <1.25 mg/I (2 samples) Total P Quarterly <0.05—0.06 mg/I (2 samples) Copper Quarterly All <0.01 mg/I (2 samples) Zinc Quarterly All 0.011 mg/I (2 samples) 4.1.c Review of Process Flows The Hubert WTP process discharge volumes, specifically total, regeneration and backwash volumes for February 1—April 21, 2022, were evaluated and compared to toxicity results during the study period. It was discussed at the January 2022 site visit that no obvious differences were apparent to ONWASA staff between the current flows from the various processes compared to 2020 and 2021 when the facility was passing toxicity. Nevertheless, daily flows from almost three (3) months were reviewed by Shealy personnel to determine variability and this evaluation is included as Table 2. The Hubert WTP lagoon system is comprised of three (3) 750,000-gallon lagoons for a total of 2,250,000 gallons of water retention. There is also an overflow lagoon that is not currently being used. Solids from Lagoon 1 have been dredged in the last several years, but dredging has not been accomplished in lagoons 2 and 3 and both have significant solids build up. The average daily flow from February, March and April 2022 was 77,422 gallons. Assuming no SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVACUATION 17 buildup of solids in any lagoons and an average daily influent flow into the lagoons of 77,422 gallons, the retention time through the system would be about 29 days. This, of course, does not include rainfall which would reduce retention time. Because of the buildup of solids in lagoons 2 and 3, it is likely that a more realistic retention time is between 14 and 20 days. Also, there is no way to determine the amount of short circuiting, if any, is happening through the system without a dye study. Reviewing the data from February, March and April 2022 indicated significant variability in the total, regeneration, and backwash flows on a daily and weekly basis. Looking at the data for total flow into the lagoon system during the three (3) months, daily flows varied from 35,500 to 142,500 gallons, and weekly flows varied from 48,286 gallons to 101,929 gallons. Monthly flow averages during this time varied less dramatically from 78,964 gallons in February, 85,613 gallons in March and 67,690 gallons in April 2022. This does not take into consideration rainfall during those months which would add additional volume to the lagoons increasing dilution but decreasing treatment retention. Since all toxicity results during February, March and April 2022 resulted in failures with similar mortality rates, there does not appear to be a significant link between flow rates and the toxicity observed. However, since it was established clearly in the previous TIE report (November 2020 TIE Report) that the Regeneration Process is by far the most toxic at the facility, it is reasonable to assume that flow rates from other processes and high rainfall could have some positive effect on toxicity simply by dilution. Solids build up in the lagoon system do not appear to be related to toxicity at the time of this study. However, compounds generated in low dissolved oxygen environments such as those that most certainly exist in the Hubert WTP lagoons with solids build up, could have a negative impact on future results. Dredging the solids from all the lagoons on a regular basis would also be beneficial in extending the retention time through the system. SHEALY v III Ill R I \\ I I' I u\I( I I IOO I:y III I( \ I I(>y I \ vI l v Ily 18 Table 2: Evaluation of Flow Data for the HWTP Process Areas from February to April 2022 Month February March April Total Plant Flow to Lagoons (GPD) Average Monthly Flow (GPD) 78,964 85,613 67,690 Lowest Daily Flow(GPD) 53,500 53,500 35,500 Highest Daily Flow (GPD) 107,000 142,500 107,000 Average Weekly Flow(GPD) -Week 1 78,874 101,929 76,143 Average Weekly Flow(GPD)-Week 2 83,786 83,857 78,643 Average Weekly Flow (GPD) -Week 3 82,143 91,643 48,286 Average Weekly Flow(GPD) -Week 4 71,071 80,150 - Difference Between Weekly Flow 15.2% 21.4% 38.6% Regeneration Flow to Lagoons (GPD) Average Monthly Flow (GPD) 46,464 54,000 35,143 Lowest Daily Flow(GPD) 18,000 18,000 18,000 Highest Daily Flow (GPD) 72,000 90,000 72,000 Average Weekly Flow (GPD) -Week 1 48,857 59,143 41,143 Average Weekly Flow (GPD)-Week 2 46,286 48,857 41,143 Average Weekly Flow (GPD) -Week 3 52,143 59,143 23,143 Average Weekly Flow(GPD) -Week 4 38,571 50,400 - Difference Between Weekly Flow 26.0% 17.4% 43.7 Backwash Flow to Lagoons (GPD) Average Monthly Flow (GPD) 32,500 31,613 35,143 Lowest Daily Flow(GPD) 0 17,500 0 Highest Daily Flow (GPD) 52,500 52,500 52,500 Average Weekly Flow (GPD) -Week 1 30,017 42,786 35,000 Average Weekly Flow (GPD) -Week 2 36,857 35,000 37,500 Average Weekly Flow (GPD)-Week 3 30,000 32,500 25,143 Average Weekly Flow(GPD) -Week 4 32,500 29,750 - Difference Between Weekly Flow 18.6% 30.5% 33.0% SHEALY v HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 19 4.1.d Review of Hubert WTP Source Water Two (2) samples of source water were collected December 20 and December 21, 2021, from the red and blue raw water taps and the individual wells on each line. From the red source water tap, samples from wells#1, #2, #4,#7, #11 and#14 were analyzed. From the blue source water tap, samples from wells#3, #6, #8,#9, #10, #12, #13 and #15 were analyzed for various inorganic constituents. The Hubert WTP draws source water from these wells and alternates the wells every other day. The results from these tests can be found in Appendix B and Table 3. Nitrate, nitrite, bromide, phosphate, and ortho-phosphate were not observed in any of the fourteen (14) well sites evaluated.TDS constituents (major and minor) measured including calcium, magnesium, potassium, iron, manganese, sodium, chloride, silicon and fluoride were all at levels normally observed for groundwater samples. Alkalinity and hardness (as CaCO3) were also at expected concentrations in groundwater close to coastal environments. No constituents measured were suspected of being at levels or close to levels that could be contributing to toxicity. 4.1.e Review of Chemicals Used at the Hubert WTP Two (2) chemicals used at the Hubert WTP were reviewed for the potential to cause toxicity, potassium permanganate and the stain removal product. It was determined with the use of Safety Data Sheets (SDS)for the products and additional research that neither of these products should be contributing to toxicity. Key information about these chemicals, references and rationale are given in Appendix C. SHEALY o I Il 111 1 I va I I Ov1( 11 II)1 v I 11 I( \ I IOy i y \I l \ I luv 20 Table 3: Analytical Results from Well Samples Collected December 2022 Parameter Results (mg/L) BLUE TAP WELLS Combined #3 #6 #8 #9 #10 #12 #13 #15 Nitrate ND ND ND ND ND ND ND ND ND Nitrite ND ND ND ND ND ND ND ND ND Bromide ND ND ND ND ND ND ND ND ND Chloride 8.83 8.86 10.1 8.45 9.21 8.34 8.38 8.35 8.78 Fluoride 0.147 0.149 0.158 0.210 0.145 0.110 0.178 0.0988 0.125 Sulfate 2.35 3.23 4.10 2.06 ND 2.62 1.42 2.59 1.64 Phosphate-P ND ND ND ND ND ND ND ND 0.0930 Sodium 5.54 5.21 5.17 5.15 9.31 4.89 5.09 5.00 5.33 Magnesium 1.24 1.23 1.14 1.12 1.95 1.39 1.03 1.12 1.33 Calcium 66.0 66.9 66.3 62.8 83.8 68.3 56.6 62.1 72.9 Potassium 0.815 0.657 0.731 0.776 1.99 0.519 0.756 0.568 0.694 Iron 0.17 0.66 0.37 0.49 0.51 0.43 0.34 0.77 0.32 Manganese 0.0690 0.0660 0.0730 0.680 0.179 0.0780 0.0640 0.0870 0.0780 Conductivity 318 317 317 299 408 323 275 295 342 (umos/cm) Alkalinity 189 185 183 180 245 193 164 169 208 Ortho-phosphate ND ND ND ND ND ND ND ND ND Silica 19.5 16.8 18.2 17.3 30.5 18.3 19.2 14.8 18.4 Hardness 170 172 170 162 217 177 146 160 188 RED TAP WELLS Combined #1 #2 #4 #7 #11 #14 Nitrate ND ND ND ND ND ND ND Nitrite ND ND ND ND ND ND ND Bromide ND ND ND ND ND ND ND Chloride 8.73 8.34 8.84 10.1 7.91 9.47 8.57 Fluoride 0.132 0.116 0.116 0.147 0.186 0.110 0.0871 Sulfate 1.51 1.40 1.07 6.17 1.15 ND 3.09 Phosphate-P ND ND ND ND ND ND ND Sodium 6.66 10.0 5.99 5.62 5.11 7.03 4.89 Magnesium 1.45 1.75 1.36 1.49 1.21 1.60 1.11 Calcium 75.0 79.0 77.6 75.0 61.8 88.4 60.1 Potassium 0.826 1.28 0.706 0.646 0.682 0.864 0.593 Iron 0.40 0.53 0.86 0.048 0.24 0.71 0.38 Manganese 0.0800 0.0900 0.109 0.0690 0.0640 0.115 0.0740 Conductivity 356 384 363 354 295 413 287 (umos/cm) Alkalinity 204 241 223 210 175 248 179 Ortho-phosphate ND ND ND ND ND ND ND Silica 21.4 26.0 21.4 18.9 16.3 26.0 15.9 Hardness 193 205 200 194 159 227 155 SHEALY 0 HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 21 4.2 Toxicity Testing Toxicity testing using the NPDES test species Amercamysis bahia (Mysid Shrimp) was conducted throughout the course of this project and all tests resulted in failures. Table 4 and Appendix D provides results from toxicity testing performed during the toxicity evaluation study. Toxicity samples were collected twice monthly during the months of March and April 2022 to obtain toxic samples on which to perform Phase I characterization testing. Water chemistry measurements taken during routine testing by the NPDES toxicity lab were minimal and offered no candidates for toxicity. Salinity for all samples was adjusted to 25 ppt with Crystal Sea Salts. Effluent samples collected for toxicity testing had initial (before adjustment) salinities ranging from 4.7 to 5.5 ppt. Table 4: Results from Toxicity Testing January— May 2022 Sample Collection Test Results Pass or Fail 1/4/22 30% Mortality Fail 2/7/22 70% Mortality Fail 3/7/22 57.5% Mortality Fail 3/21/22 31.6% Mortality Fail 4/4/22 62.5% Mortality Fail 4/17/22 72.5% Mortality Fail 5/2/22 72.5% Mortality Fail 4.3 Toxicity Persistence Testing The sample collected February 7, 2022, was initially tested, and found to be acutely toxic (70% mortality). To determine the degree of toxicity persistence the sample was held for eleven (11) days and retested for toxicity. After that time period the sample remained similarly toxic (65% mortality). The fact that toxicity was persistent was one of the reasons that ionic imbalances or high ions was suspected as potentially playing a part in toxicity since this condition would be persistent over time. SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 4.4 Identification of Lagoon Algae There was a concern for toxic by-products by the algae build-up in Lagoons 2 and 3 at the Hubert WTP. As a result, a sample was collected May 2, 2022, and sent to the Clemson University Plant and Pest Diagnostic Clinic. Results from those analyses are given in Appendix E and indicated that there were several species of green algae present, none of which would have toxic by-products. 4.5 Analytical Testing on Effluent A total of eight (8) samples were collected for analytical testing between March 8 and April 26, 2022. The range of results from these tests are provided in Table 5. For many of the analytes, including cations and anions, samples were tested with and without salt adjustment to 25 ppt, the toxicity test salinity. Most of the metals and all heavy metals that typically cause toxicity in effluents (Copper, Zinc, Nickel, Cadmium) were at concentrations well below toxic thresholds. Nitrogen compounds including ammonia, nitrate and nitrite were all below detection limits. From the beginning of the study there was a concern that ionic imbalances may be contributing to toxicity. Toxicity of effluent with atypical ion concentrations and ratios to freshwater organisms has been studied by several researchers; however, fewer data exist on ion toxicity to marine organisms. Although adverse effects may be associated with general osmotic factors, the importance of individual ions to specific physiologic activities are probably more important. The breakdown of major ion components in the Hubert WTP effluent after salt adjustment to 25 ppt (the toxicity test salinity) was compared to major ions in typical seawater at 25 ppt. This comparison is provided in Table 6. Ions present in Hubert effluent samples at comparable levels to 25ppt saltwater were bromide, chloride, sulfate, potassium, sodium, and strontium. The high end of the fluoride range (2.94 mg/I) was significantly higher than the average for seawater at 25 ppt but fluoride is not toxic to Mysid Shrimp at this level based on previous Shealy lab experiments. In addition, Hubert effluent samples collected during the study period that contained little or no fluoride were also found to be toxic. Calcium was consistently observed in the eight (8) samples tested to be 3-4 times high than seawater. SHEALY �� i vt � , !t ! � �I „ II I�_ �. _ I� �'. 'vI l `�. II( 23 //- Table 5: Results from Analytical Testing (Except Metals) on Effluent Samples Collected March and April 2022 Parameter Range of Range of Parameter Range of Concentrations Concentrations Concentrations Observed(mg/L) Observed (mg/L) Observed(mg/L) Unadjusted Salinity adjusted Unadjusted to 25 ppt Nitrate All<DL <DL-1.6 Aluminum <DL-0.021 Nitrite <DL-0.005 All<DL Antimony 0.012-0.017 Bromide All<DL 41.8—51.4 Arsenic All<DL Chloride 1990-3020 13,100—15,000 Barium 0.049—0.059 Fluoride <DL—1.44 <DL—2.94 Beryllium All<DL Sulfate 12.9—21.1 1780-2100 Boron <DL—0.018 Phosphate-P All<DL <DL-10.5 Cadmium All<DL Calcium 646-976 993-1260 Cobalt All<DL Magnesium 12.3—19.0 653-769 Copper All<DL Potassium 11.4—18.2 207-243 Iron 0.013—0.141 Sodium 537-886 6130-7320 Lead All<DL Salinity 4.6—5.7 ppt All 25 ppt Manganese 0.018—19.8 pH 7.76—7.99 8.28—8.55 _Molybdenum All<DL Alkalinity, 93.5- 119 60- 174 Nickel All<DL CaCo3 Bicarbonate as 92.8-119 60- 151 Selenium All<DL CaCO3 Ammonia-N All< DL All<DL Silver All<DL Total hardness 1660-2520 5300-6220 Selenium All<DL TDS 5600-6550 - Strontium 2.83—2.92 TSS 1.9—3.4 - Thallium All< DL Tin 0.015—0.057 Titanium All< DL Vanadium All<DL Zinc <DL-0.012 SHEALY o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 24 Table 6: Results from Major Ion Components of Salt Adjusted Effluent Compared to Seawater Parameter Range of Concentrations Observed Typical (mg/L)in Hubert WTP Effluent with Seawater at 25 salinity adjusted to 25ppt ppt Bromide 41.8—51.4 49 Chloride 13,100—15,000 14,425 Fluoride <DL-3.02 0.076 Sulfate 1780-2100 2013 Calcium 993- 1260 304 Magnesium 653-769 957 Potassium 207-243 289 Sodium 6130-7320 8023 Bicarbonate as CaCO3 60- 151 106 Strontium 10.24—10.33* 9.9 *Strontium not analyzed on salt adjusted effluent so known concentrations from Crystal Sea Salts added to concentrations observed in unadjusted effluent samples. In addition to the analyses of ions,the balance of ions for two (2) toxic samples collected March 7- 8, 2022 and April 4-5, 2022, were evaluated with results provided in Tables 7 and 8. The ion balances calculated for toxic Hubert samples collected March 7-8 and April 4-5 were 6.85% and 7.02%, respectively. These were the samples used for the Phase I toxicity characterization experiments. In one study(Pillard, et.al), models were developed for mysid shrimp toxicity to ion imbalances and found that the organisms survived well after 48 hours in a solution that had a 14% excessive positive charge (Ion Imbalance). Since the imbalances calculated for the two (2) Hubert effluent samples were about half the reported ionic imbalance threshold reported from this study it was not thought that ionic imbalance was the culprit for toxicity, although it was believed that it might be contributing. In addition, the results reported from the Pillard study were for a 48-hour exposure period and the Hubert NPDES toxicity test exposure period is 24 hours. It would be reasonable to expect that higher imbalance ratios than 14% might be needed to cause the acute toxicity after 24 hours routinely observed for the Hubert WTP effluent. SHEALY o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 25 Table 7: Ion Balance for Effluent Collected March 7-8, 2022 with Salinity adjusted to 25 ppt Parameter Concentration Molecular Valence mEq/L* Mg/L Weight(MW) CATIONS Calcium 1140 40.08 +2 56.89 Sodium 7080 22.99 +1 308.0 Magnesium 692 24.31 +2 35.41 Potassium 235 39.09 +1 6.01 Strontium** 10.3 87.62 +2 0.24 ECations 406.6 ANIONS Chloride 15000 35.45 -1 423.1 Sulfate 2000 96.06 -2 41.64 Bicarbonate 60 61.02 -1 0.98 Bromide 47.4 79.90 -1 0.59 Fluoride 1.69 19.0 -1 0.09 Z Anions 466.4 Ion Balance*** -6.85% * mEq = mg substance/MW x Valence ** Strontium not analyzed on salt adjusted effluent so known concentrations from Crystal Sea Salts added to concentrations observed in effluent. *** Ion Balance calculated as ECations— EAnions/Total Ions SHEA o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 2(1 Table 8: Ion Balance for Effluent Collected April 4-5, 2022, with Salinity adjusted to 25 ppt Parameter Concentration Molecular Valence mEq/L* Mg/L Weight(MW) CATIONS Calcium 993 40.08 +2 49.55 Sodium 6470 22.99 +1 281.4 Magnesium 686 24.31 +2 56.44 Potassium 220 39.09 +1 5.62 Strontium** 10.26 87.62 +2 0.23 E Cations 393.2 ANIO NS Chloride 14400 35.45 -1 406.2 Sulfate 2100 96.06 -2 43.72 Bicarbonate 142 61.02 -1 2.33 Bromide 51.4 79.90 -1 0.64 Fluoride 2.94 19.0 -1 0.15 E Anions 453.0 Ion Balance*** -7.07% * mEq = mg substance/MW x Valence ** Strontium not analyzed on salt adjusted effluent so known concentrations from Crystal Sea Salts added to concentrations observed in effluent. *** Ion Balance calculated as ECations— E Anions/Total Ions As previously mentioned, calcium concentrations in Hubert WTP effluent were consistently three (3) to four(4) times higher than seawater at the same salinity. Unfortunately,there is no calcium data samples collected during 2020 and 2021 that were passing toxicity. Since calcium is a cation and has positive charge, the excess of this constituent is not responsible for the ionic imbalance in the effluent. Rather,the relatively low concentrations of sodium (compared to seawater at comparable salinity) is likely the culprit for excess negative charge in the effluent. SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 27 A literature search indicated that excess calcium has been found to be toxic to Mysid Shrimp (Douglas, et al; Kline, ER and Stekoll, MS; Goodfellow, et al) at the levels observed in Hubert effluent. The upper limit for the toxic threshold (no observed effect concentration, NOEC for acute toxicity) for calcium at 25 ppt for Mysid Shrimp has been found to be approximately 600 mg/I. Concentrations observed for this study ranged from 646 mg/I —976 mg/I in the effluent without salt addition and 993 mg/I — 1260 mg/I in effluent with salt adjusted to 25 ppt for testing. Typical seawater at 25ppt contains approximately 300 mg/I of calcium. It is believed that high calcium concentrations are contributing to toxicity. 4.6 Phase I Toxicity Characterization Results To characterize the toxicant(s) present in the Hubert WTP effluent samples, a battery of toxicity characterization tests was performed on two (2) samples previously found to be toxic. Tables 9 and 10 provide the results from Phase I toxicity characterization testing performed for this project. Bench data can be found in Appendix F. Two samples, both comparably toxic were chosen to be tested, one collected March 7-8, 2022 and one collected April 4-5, 2022. Both samples were put through the series of manipulations and then salt adjusted to 25 ppt prior to testing. For the sample collected March 7-8, 2022, no manipulations improved toxicity. From experience and the literature (Goodfellow, et. al)this would be the expected result if ionic imbalances were in play. The ion imbalance for this effluent was 6.85%. However,the calcium concentration of this sample was 1140 mg/I, significantly above reported toxic thresholds for Mysid Shrimp. EDTA does chelate with calcium, but it forms a weak bond (USEPA, 1991) and therefore, it is possible that the toxicity was associated with the calcium and not ionic imbalance, but it is impossible to know for sure with these data. SHEALY OyII 11 l IDI `v Il! i( \ I !Ov Lv vI ! v !lOy 28 Table 9: Results from Phase I Characterization Testing on Effluent Collected March 8, 2022 Manipulation % Mortality after 24 hours Significant Improvement? Control 0 - Untreated w/salt 50 - adjustment Untreated - no salt 100 - adjustment pH3 100 No pH11 80 No Aerated pHi 70 No Aerated pH3 90 No Aerated pH11 100 No Filtered pHi 70 No Filtered pH3 100 No Filtered pH11 80 No C18 SPE pHi 100 No C18 SPE pH3 80 No C18 SPE pH9 40 No EDTA 19 mg/I 80 No EDTA 38 mg/I 70 No EDTA 75 mg/I 60 No EDTA 150 mg/I 70 No EDTA 300 mg/I 60 No Ox Redox 6.3 mg/I 80 No Ox Redox 12.5 mg/I 70 No Ox Redox 25 mg/I 70 No Ox Redox 50 mg/I 60 No Ox Redox 100 mg/I 90 No Blank-Aeration 0 - Blank- Filtration 0 - Blank—C18SPE 0 - All Solutions adjusted to 25 ppt SHEALY o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 29 Table 10: Results from Phase I Characterization Testing on Effluent Collected April 5, 2022 Manipulation % Mortality after 24 hours Significant Improvement? Control 0 - Untreated w/salt 70 - adjustment Untreated - no salt 100 - adjustment pH3 85 No pH11 45 No Aerated pHi 70 No Aerated pH3 35 No Aerated pH11 65 No Filtered pHi 75 No Filtered pH3 65 No Filtered pH11 80 No C18 SPE pHi 75 No C18 SPE pH3 65 No C18 SPE pH9 50 No EDTA 19 mg/I 65 No EDTA 38 mg/1 30 Some EDTA 75 mg/I 30 Some EDTA 150 mg/1 30 No EDTA 300 mg/I 15 Yes Ox Redox 6.3 mg/I 80 No Ox Redox 12.5 mg/I 75 No Ox Redox 25 mg/I 70 No Ox Redox 50 mg/I 45 No Ox Redox 100 mg/I 70 No Blank-Aeration 0 - Blank- Filtration 0 - Blank—C18SPE 0 - All Solutions adjusted to 25 ppt gtEA Y o HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 30 For the sample collected April 4-5, 2022, the same manipulations were performed. For this sample the highest EDTA concentration of 300 mg/L reduced toxicity from 70% in the untreated sample to 15%which is significant. The calcium concentration of this sample was 993 mg/I which was lower than the 1140 mg/I observed for the sample collected March 7-8, 2022. As mentioned before, EDTA does form a bond (albeit a weak one) with calcium, so it is possible that the EDTA concentration range was not high enough to chelate the calcium in the March 7- 8 sample. As previously mentioned, there were no other cationic metals present in the effluent samples that might be toxic to the Mysid Shrimp and be chelated by EDTA other than calcium and therefore, it is believed that calcium was responsible for the toxicity in this sample. SHEALY •v HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 31 SECTION 5.0 CONCLUSIONS The TIE was completed late May 2022 and the following conclusions were made as a result of the study: ✓ As a part of the TIE process, past effluent analytical data (January —June 2020) for the Hubert WTP had been previously provided to Shealy for review. The analytical data from 2020 represented samples collected during a period in which toxicity passes and failures had been observed. It was previously determined that no obvious candidates for toxicity were identified with the available data and this opinion remained during this project. ✓ The Dixon WTP which has a similar process as the Hubert WTP but also has RO treatment, consistently meets toxicity limits. As a result, analytical data from one sample collected February 2022 from the Dixon WTP was compared to data from the Hubert WTP collected the same day. The data from this testing indicated that the Hubert WTP effluent contained significantly higher concentrations of bromide, calcium, chloride, iron, magnesium, manganese, sodium, and sulfate than the Dixon WTP effluent. ✓ The Hubert WTP process discharge volumes, specifically total, regeneration and backwash flows for February 1 —April 21, 2022, were evaluated and compared to toxicity results during the study period. It was discussed at a January 2022 site visit that no obvious differences were apparent to ONWASA staff between the current flows from the various processes compared to 2020 and 2021 when the facility was passing toxicity. Nevertheless, daily flows from almost three (3) months were reviewed by Shealy personnel to determine variability. The Hubert WTP lagoon system is comprised of three (3) 750,000-gallon lagoons for a total of 2,250,000 gallons of water retention. Solids from Lagoon 1 have been dredged in the last several years, but dredging has not been accomplished in lagoons 2 and 3 and both have significant solids build up. SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION Reviewing the data from February, March and April 2022 indicated significant variability in the total, regeneration, and backwash flows on a daily and weekly basis.This does not take into consideration rainfall during those months which would add additional volume to the lagoons increasing dilution but decreasing treatment retention. Since all toxicity results during February, March and April 2022 resulted in failures with similar mortality rates, there does not appear to be a significant link between flow rates and the toxicity observed. However, since it was established clearly in the previous TIE report (November 2020 TIE Report) that the Regeneration Process is by far the most toxic at the facility, it is reasonable to assume that flow rates from other processes and high rainfall could have some positive effect on toxicity simply by dilution. ✓ Solids build up in the lagoon system do not appear to be related to toxicity at the time of this study other than reducing retention time in the treatment lagoons. However, compounds generated in low dissolved oxygen environments such as those that most certainly exist in the Hubert WTP lagoons with solids build up, could have a negative impact on future results. Dredging the solids from all the lagoons on a regular basis would also be beneficial in extending the retention time through the system. ✓ Two (2) samples of source water were collected December 20 and December 21, 2021, from the red and blue raw water taps and the individual wells on each line. No constituents measured were suspected of being at levels or close to levels that could be contributing to toxicity. ✓ Two (2) chemicals used at the Hubert WTP were reviewed for the potential to cause toxicity, potassium permanganate and the stain removal product. It was determined with the use of Safety Data Sheets (SDS) for the products and additional research that neither of these products should be contributing to toxicity. ✓ A sample collected February 7, 2022, was initially tested for toxicity, and found to be acutely toxic (70% mortality). To determine the degree of toxicity persistence the SHEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 33 sample was held for eleven (11) days and retested for toxicity. After that time period the sample remained similarly toxic (65% mortality). The fact that toxicity was persistent was one of the reasons that ionic imbalances or high ions was suspected as potentially playing a part in toxicity since this condition would be persistent over time. ✓ There was a concern for toxic by-products by the algae build-up in Lagoons 2 and 3 at the Hubert WTP. As a result, a sample was collected May 2, 2022, and sent to the Clemson University Plant and Pest Diagnostic Clinic. Results from those analyses indicated that there were several species of green algae present, none of which would have toxic by-products. ✓ A total of eight (8) samples were collected for analytical testing between March 8 and April 26, 2022. For many of the analytes, including cations and anions, samples were tested with and without salt adjustment to 25 ppt, the toxicity test salinity. Most of the metals and all heavy metals that typically cause toxicity in effluents (Copper,Zinc, Nickel, Cadmium)were at concentrations well below toxic thresholds. Nitrogen compounds including ammonia, nitrate and nitrite were also all below detection limits. ✓ From the beginning of the study there was a concern that ionic imbalances may be contributing to toxicity. The breakdown of major ion components in the Hubert WTP effluent after salt adjustment to 25 ppt (the toxicity test salinity)was compared to major ions in typical seawater at 25 ppt. Ions present in Hubert effluent samples at comparable levels to 25 ppt saltwater were bromide, chloride, sulfate, potassium, sodium, and strontium. Fluoride and calcium were consistently observed in the samples higher than seawater. ✓ The high end of the fluoride range (2.94 mg/I) observed in effluents was significantly higher than the average for seawater at 25 ppt. Fluoride is not toxic to Mysid Shrimp at this level based on previous Shealy lab experiments. In addition, Hubert effluent samples collected during the study period that contained little or no fluoride were also found to be toxic. SHEALY o III III IZI \\ I I' I O\I( 1 1 1 11)1 yIII I( \ I I()v I y \I I v IIOy 34 ✓ Ions were measured for two (2) toxic samples and the ion imbalances calculated. It was believed that the relatively low concentrations of sodium (compared to seawater at comparable salinity) was likely the culprit for excess negative charge in the effluent. Because the imbalances calculated were about half the threshold for toxicity reported in the literature, it was not thought that ionic imbalance was the culprit for toxicity, although it is believed that it might be contributing. ✓ Calcium concentrations in Hubert WTP effluent were consistently three (3)to four(4) times higher than seawater at the same salinity. Unfortunately, there is no calcium data for samples collected during 2020 and 2021 that were passing toxicity. Concentrations observed for this study ranged from 646 mg/I —976 mg/I in the effluent without salt addition and 993 mg/I —1260 mg/I in effluent with salt adjusted to 25 ppt for testing. Typical seawater at 25 ppt contains approximately 300 mg/I of calcium. ✓ A literature search indicated that excess calcium has been found to be toxic to Mysid Shrimp at the levels observed in Hubert effluent and lower. The upper limit for the toxic threshold (no observed effect concentration, NOEC for acute toxicity) for calcium at 25 ppt for Mysid Shrimp has been reported as being approximately 600 mg/I. It is believed that high calcium concentrations were contributing to toxicity in the Hubert WTP effluent and was the major contributor during the study. ✓ Phase I toxicity characterization testing performed on a sample collected April 4-5, 2022, confirmed the conclusion that calcium was a major contributor of toxicity during the study. For this sample EDTA which forms a complex with calcium, reduced toxicity from 70% in the untreated sample to 15%which is significant. The calcium concentration of this sample was 993 mg/I, above the reported toxic threshold. HEALY HUBERT WTP TOXICITY IDENTIFICATION EVALUATION 35 REFERENCES Douglas, WS and Horne, MT. 1996. The Interactive Effects of Essential Ions and Salinity on the Survival of Mysidopsis bahia in 96-Hour Acute Toxicity Tests of Effluents Discharged to Marine and Estuarine Receiving Waters. Environmental Toxicology and Chemistry, Vol. 16, No. 10. Goodfellow, et al. 1999. Major Ion Toxicity in Effluents:A Review with Permitting Recommendations. Environmental Toxicology and Chemistry, Vol. 11. Hobbs, et al. 2006. Comparative acute toxicity of potassium permanganate to nontarget Aquatic organisms. Environmental Toxicology and Chemistry, Vol. 11. Kline, ER and Stekoll, MS. 1999. The Role of Calcium and Sodium in Toxicity of An Effluent to Mysid Shrimp. Environmental Toxicology and Chemistry, Vol. 19. Pillard, David L. et al. 2001. Development and Validation of Models Predicting the Toxicity of Major Seawater Ions to the Mysid Shrimp,Americamysis bahia. Environmental toxicology and Chemistry. Vol. 21, No. 10. USEPA, 1991. Methods for Aquatic Toxicity Identification Evaluations, Second Edition. (EPA/600/6-91/003). USEPA, 1999. Toxicity Reduction Evaluation Guidance for Municipal Wastewater Treatment Plants. EPA 833-8-99-002. Office of Wastewater Management, Washington, D.C. USEPA, 2001. Clarifications Regarding Toxicity Reduction and Identification Evaluations in the National Pollutant Discharge Elimination System Program, Washington, DC. USEPA, 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA 821-R-02-012. Environmental Research Laboratory, Duluth, MN. ea o HUBERT WTP TOXICITY IDENTIFICATION EVALUATIU\ 36 APPENDIX A DW Matrix Comparison 2/14/2022 WW%DIFF represents wastewater effluent differences of HWTP when compared to DWTP.Positive percent equals more than Bromide mg/L 0 0.526 100% DWTP and negative percent equals less than OWTP. Overall,HWTP has almost 30%more calcium,chloride,iron,and sodium than Calcium mg/L 435 907 35% DWTP does in the WW effluent. Chloride mg/L 1450 2860 33% Conductivity uS/cm 4240 8170 32% Iron mg/L 0.027 0.048 28% Magnesium mg/L 27.1 17.3 -22% Manganese mg/L 0.107 0.164 21% pH pH Units 8.01 7.9 -1% Potassium mg/L 20.4 18.6 -5% Silica mg/L 54 13 -60% Sodium mg/L 456 780 26% Sulfate mg/L 1.22 2.99 42% Total Hardness mg/L n/a n/a n/a RAW %DIFF represents raw source water Bromide mg/L 0.02 0.00 0.00 0.00 0.01 0.00 -100% differences of HWTP when compared to DWTP. Calcium mg/L 85 83 62 78 84 70 -9% Positive percent equals more than DWTP and Chloride mg/L 14 14 9 9 14 9 -23% negative percent equals less than DWTP. Overall, Conductivity uS/cm 396 397 313 350 396 331 -9% HWTP has 25% less ions than DWTP coming into Iron mg/L 0.28 0.24 0.15 0.29 0.26 0.22 -8% the plant for treatment Magnesium mg/L 4.21 4.13 0.79 1.07 4.17 0.93 -63% Manganese mg/L 0.10 0.15 0.04 0.06 0.12 0.05 -42% pH pH Units 7.55 7.48 7.52 7.34 7.52 7.43 -1% Potassium mg/L 3.34 2.59 1.13 0.93 2.97 1.03 -48% Silica mg/L 54 55 18 20 55 19 -48% Sodium mg/L 11 13 14 7 12 10 -9% Sulfate mg/L 0.38 1.25 2.92 2.34 0.82 2.63 53% Total Hardness mg/L 1 230 225 159 198 227 179 -12% "A"AVG "F"AVG A&F%DIFF A&F%DIFF represents distribution sites solely Bromide mg/L 0.00 0.00 0.00 0.00 0.00 0.00 0% influenced by each treatment plant. HWTP sites Calcium mg/L 26 27 25 25 26 25 -1% F17&F46 when compared to DWTP sites A19& Chloride mg/L 20 20 11 11 20 11 -28% A20.Positive percent equals more than DWTP and Conductivity uS/cm 407 407 314 311 407 313 -13% negative percent equals less than DWTP. Overall, Iron mg/L 0.01 0.02 0.05 0.02 0.01 0.03 39% HWTP has 12%less ions than DWTP going out into Magnesium mg/L 0.94 1.00 0.00 0.00 0.97 0.00 -100% the potable distribution system. Manganese mg/L 0.02 0.03 0.07 0.02 0.02 0.05 34% pH pH Units 7.46 7.48 7.59 7.59 7.47 7.59 1% Potassium mg/L 2.56 2.62 1.16 1.16 2.59 1.16 -38% Silica mg/L 52 50 19 19 51 19 -46% Sodium mg/L 76 74 68 67 75 67 -5% Sulfate mg/L 0.00 0.00 0.00 0.00 0.00 0.00 0% Total Hardness mg/L 68 70 64 64 69 64 -4% WW%DIFF AVG 29% RAW%DIFF AVG -25% A&F%DIFF AVG -12% ONWASA Laboratory 228 Georgetown Road Jacksonville,NC 28540 Ion Balance 2/14/2022 Hubert WTP Effluent Dixon WTP Effluent Measured Formula ' Calculated Measured Formula Calculated Cation Valence Cation Valence Conc mg/L Wt g meq/L Conc mg/L Wt g meq/L Ca 2+ 907 40.08 2 45.26 Ca 2+ 435 40.08 2 21.71 Mg 2+ 17.3 24.31 2 1.42 Mg 2+ 27.1 24.31 2 2.23 Na+ 780 23 1 33.91 Na+ 456 23 1 19.83 K+ 18.6 39.1 1 0.48 K+ 20.4 39.1 1 0.52 _ Fe 2+ 0.048 55.85 2 0.00 Fe 2+ 0.027 55.85 2 0.00 Mn 2+ 0.164 54.92 2 0.01 Mn 2+ 0.107 54.92 2 0.00 Cation Sum 81.08 Cation Sum 44.29 Measured Formula Calculated Measured Formula Valence Calculated Anion Valence Anion Conc mg/L Wt g meq/L Conc mg/L Wt g meq/L HCO3 133 61.02 -1 2.18 HCO3 198 61.02 -1 3.24 Cl- 2860 35.45 -1 80.68 CI- 1450 35.45 -1 40.90 NO3 0 62 -1 0.00 NO3 0 62 -1 0.00 S042- 2.99 96.06 -2 0.06 S042 1.22 96.06 -2 0.03 P03 3 0 95 -3 0.00 P03 3 0 95 -3 0.00 F 0 19 -1 0.00 F- 0.129 19 -1 0.01 Si024 13.2 60.08 -4 0.88 Si024 53.6 60.08 -4 3.57 Anion Sum 83.80 Anion Sum 47.75 5%or less demostrates balance 5%or less demostrates balance Cation Anion Balance -1.6% Cation Anion Balance -3.8% ION ,,. Cation 29% 81 44 Anion 27% 84 48 1 ONWASA Laboratory 228 Georgetown Road Jacksonville, NC 28540 C. ONWASA ONWASA Special Project Project: DW Plants Effluent Study 228 Georgetown Road Project Number: Reported: Jacksonville,NC 28540 Project Manager: Todd A Roberts 02/14/2022 13:38 Sample Results Sample: Dixon Effluent Composite L220702-01 (WW) D220601-01A-aliquot was taken from this sample to conduct this analysis. Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate <0.00900 1.00 mg/L 02/08/2022 DMK EPA 300.1 Nitrite <0.00200 0.100 mg/L 02/08/2022 DMK EPA 300.1 Bromide <0.0580 0.250 mg/L 02/08/2022 DMK EPA 300.1 Fluoride 0.129 0.250 mg/L 02/08/2022 DMK EPA 300.1 Sulfate 1.22 5.00 mg/L 02/08/2022 DMK EPA 300.1 Phosphate-P <0.0690 0.250 mg/L 02/08/2022 DMK EPA 300.1 Calcium 435 10.0 mg/L 02/09/2022 DMK EPA 300.1 Magnesium 27.1 2.50 mg/L 02/09/2022 DMK EPA 300.1 Potassium 20.4 5.00 mg/L 02/09/2022 DMK EPA 300.1 Sodium 456 50.0 mg/L 02/09/2022 DMK EPA 300.1 Chloride 1450 5.00 mg/L 02/10/2022 TAR SM 4500 CLDE-E Iron 0.0270 0.0500 mg/L 02/08/2022 DMK EPA 199 A Rev 1 Manganese 0.107 0.0500 mg/L 02/08/2022 DMK SM 3500 Mn D Conductivity 4240 uS/cm 02/09/2022 DMN SM 2510 B pH 8.01 pH Units 02/09/2022 DMN SM 4500 H B Alkalinity,CaCO3 198 mg/L 02/09/2022 DMN EPA 310.1 Silica 53.6 1.00 mg/L 02/09/2022 DMK SM 4500 P E Total Dissolved Solids 2940 2.50 mg/L 02/04/2022 TAR SM 2540 C Sample: Hubert Effluent Composite L220702-02 (WW) H220701-01A aliquot was taken from this sample to conduct this analysis. Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate <0.00900 1.00 mg/L 02/08/2022 DMK EPA 300.1 Nitrite <0.00200 0.100 mg/L 02/08/2022 DMK EPA 300.1 Bromide 0.526 0.250 mg/L 02/08/2022 DMK EPA 300.1 Fluoride <0.0660 0.250 mg/L 02/08/2022 DMK EPA 300.1 Sulfate 2.99 5.00 mg/L 02/08/2022 DMK EPA 300.1 Phosphate-P <0.0690 0.250 mg/L 02/08/2022 DMK EPA 300.1 Calcium 907 10.0 mg/L 02/09/2022 DMK EPA 300.1 I Magnesium 17.3 2.50 mg/L 02/09/2022 DMK EPA 300.1 Potassium 18.6 5.00 mg/L 02/09/2022 DMK EPA 300.1 Sodium 780 50.0 mg/L 02/09/2022 DMK EPA 300.1 Chloride 2860 5.00 mg/L 02/10/2022 TAR SM 4500 CLDE-E Iron 0.0480 0.0500 mg/L 02/08/2022 DMK EPA 149 A Rev 1 Manganese 0.164 0.0500 mg/L 02/08/2022 DMK SM 3500 Mn D Conductivity 8170 uS/cm 02/09/2022 DMN SM 2510 B pH 7.90 pH Units 02/09/2022 DMN SM 4500 H B Alkalinity,CaCO3 133 mg/L 02/09/2022 DMN EPA 310.1 Silica 13.2 1.00 mg/L 02/09/2022 DMK SM 4500 P E Total Dissolved Solids 5900 2.50 mg/L 02/10/2022 TAR SM 2540 C The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 2 of 3 o 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Sep'16 Oct'16 Nov'16 Dec'16 Jan'17 Feb'17 Mar'17 „.......=' Apr'17 May'17 ill Jun'17 Jul'17 r Aug'17 Sep'17 Oct'17 Nov'17 Dec'17 Jan'18 Feb'18 Mar'18 Apr'18 May'18 Jun'18 .:, '- Jul'18 MOIL Aug'18 Sep'18 • Oct'18 v I Nov'18 rnn C Dec'18 mow mommummummi °' CT 01, Jan'19 fD N Feb'19 E -, Mar'19 o r... Apr'19 S May'19 ` 0 Jun'19 m Jul'19 c Aug'19 Sep'19 Oct'19 • Nov'19 Dec'19 Jan'20 Mir ..— Feb'20 Ann' 111ANNOMENIMMOMME••••••= Mar'20 Apr'20 May'20 Jun'20 _ , ., - Jul'20 Aug'20 7 Sep'20 0 Oct'20 IMMININIMI -, Nov'20 m Dec'20 D Jan'21 ao Feb'21 0, Mar'21 ler a Apr'21 °, May'21 Jun'21 r Jul'21 Aug'21 Sep'21 Oct'21 AlliMENNIIIMMill Nov'21 .. Dec'21 Jan'22 • 0 00 00 00 00 00 00 0 00 0 0 0 0 0 0 0 0 b b b 0 0 0 0 0 0 Apr'16 Aug'16 Sep'16 Oct'16 Nov'16 ANNIMMINEMERN Dec'16 Jan'17 Feb'17 MO Mar'17 Apr'17 II May'17 Jun'17 ,.-.� ;,. Jul'17 �� UMW Aug'17 Sep17 . . ,,. ..1 Oct'17 Nov'17 1 Dec'17 ` Jan'18 .111111 Feb'18 Mar'18 Apr'18 May'18 m Jun'18 Jul'18 Aug'18 ' Sep'18 r '1 • 0 Oct'18 '- Nov'18 < X. Dec'18 0 Jan'19 o M Feb'19 —I Mar'19 Apr'19 fD 0 May'19 R V) Jun'19 Jul'19 Aug'19 _ Sep'19 Oct'19 Nov'19 Dec'19 Jan'20 Feb'20 Mar'20 Apr'20 May'20 , Jun'20 Jul'20 Aug'20 Sep'20 0 Oct'20 _ 71 71• Nov'20 m Dec'20 Jan'21 _ off° Feb'21 �,, Mar'21 -. Apr'21 IIIIMMIIINIENNI °O May'21 Jun'21 11=1111111111111111111M11 r. Jul'21 INIMMINNINIMEMENIEN Aug'21 ._ _ Sep'21 Oct'21 MIN Nov'21 as Dec'21 ANIIIIIIMMINIMIMININ Jan'22 -4-411 APPENDIX B ONWASA Laboratory 228 Georgetown Road Jacksonville NC 28540 NWASA (910) 389-8511 January 12, 2022 James Arnold Hubert WTP 374 Hubert Boulevard Hubert, NC 28539 RE: Hubert Source Water Red Enclosed are the results of analyses for samples received by our laboratory on 12/21/2021. If you have any questions concerning this report, please feel free to contact me. Sincerely,‹eptie Todd A. Roberts For James Arnold Hubert Water Treatment Plant Supervisor Table of Contents Cover Letter 1 Samples in Report 3 Sample Results 4 Quality Assurance Results 8 Qualifiers and Definitions 16 Chain of Custody PDF 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Samples in this Report Lab ID Sample/Location Matrix Date Sampled Date Received H215203-01 HWTP Raw Red Tap 1 Wells 1,2,4,7,11,14 DW 12/20/2021 12/21/2021 H215203-02 HWTP Well#1 Hubert Well#1 DW 12/20/2021 12/21/2021 H215203-03 HWTP Well#11 Hubert Well#11 DW 12/20/2021 12/21/2021 H215203-04 HWTP Well#14 Hubert Well#14 DW 12/20/2021 12/21/2021 H215203-05 HWTP Well#2 Hubert Well#2 DW 12/20/2021 12/21/2021 H215203-06 HWTP Well#4 Hubert Well#4 DW 12/20/2021 12/21/2021 H215203-07 HWTP Well#7 Hubert Well#7 DW 12/20/2021 12/21/2021 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 3 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results Sample: HWTP Raw Red Tap 1 H215203-01 (DW) Wells 1,2,4,7,11,14 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.73 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.132 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 1.51 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 6.66 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.45 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 75.0 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.826 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.40 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0800 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 356 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 204 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 21.4 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 193 7.05 mg/L 01/04/2022 DMK Calculated Sample: HWTP Well #1 H215203-02(DW) Hubert Well#1 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.34 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.116 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 1.40 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 10.0 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.75 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 79.0 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 1.28 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.53 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0900 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 384 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 241 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 26.0 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 205 7.05 mg/L 01/05/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 4 of 17 44 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #11 H215203-03(DW) Hubert Well#11 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 9.47 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.110 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate ND 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 7.03 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.60 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 88.4 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 0.864 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.71 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.115 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 413 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 248 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 26.0 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 227 7.05 mg/L 01/05/2022 DMK Calculated Sample: HWTP Well #14 H215203-04(DW) Hubert Well#14 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.57 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.0871 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 3.09 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 4.89 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.11 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 60.1 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 0.593 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.38 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0740 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 287 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 179 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 15.9 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 155 7.05 mg/L 01/05/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 5 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #2 H215203-05(DW) Hubert Well#2 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.84 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.116 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 1.07 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.99 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.36 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 77.6 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 0.706 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.86 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.109 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 363 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 223 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 21.4 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 200 7.05 mg/L 01/05/2022 DMK Calculated Sample: HWTP Well #4 H215203-06(DW) Hubert Well#4 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 10.1 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.147 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 6.17 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.62 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.49 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 75.0 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 0.646 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.48 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0690 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 354 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 210 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 18.9 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 194 7.05 mg/L 01/05/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 6 of 17 A. ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #7 H215203-07(DW) Hubert Well#7 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 7.91 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.186 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 1.15 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.11 10.0 mg/L 01/05/2022 DMK EPA 300.1 Magnesium 1.21 0.500 mg/L 01/05/2022 DMK EPA 300.1 Calcium 61.8 2.00 mg/L 01/05/2022 DMK EPA 300.1 Potassium 0.682 1.00 mg/L 01/05/2022 DMK EPA 300.1 Iron 0.24 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0640 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 295 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 175 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 16.3 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 159 7.05 mg/L 01/05/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 7 of 17 A. ONWASA Hubert VV7P Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control *** DEFAULT GENERAL METHOD *** Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B215377-No Prep- Wet Chem Blank(B215377-BLK1) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 10.2 mg/L Conductivity 4.00 uS/cm Blank(B215377-BLK2) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 10.2 mg/L Conductivity 3.00 uS/cm Blank(B215377-BLK3) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 10.3 mg/L Conductivity 3.00 uS/cm LCS(B215377-BS1) Prepared&Analyzed: 12/21/2021 pH 9.76 pH Units 90-110 Alkalinity,CaCO3 247 mg/L 250 98.9 90-110 Conductivity 531 uS/cm 90-110 LCS(B215377-BS2) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 244 mg/L 250 97.4 90-110 pH 9.71 pH Units 90-110 Conductivity 488 uS/cm 90-110 LCS(B215377-BS3) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 247 mg/L 250 98.9 90-110 pH 9.68 pH Units 90-110 Conductivity 487 uS/cm 90-110 Duplicate(B215377-DUP1) Source:H215203-01 Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 215 mg/L 204 5.05 20 Hydroxide as CaCO3 ND 1.00 mg/L ND 20 Conductivity 358 uS/cm 356 0.560 20 pH 7.52 pH Units 7.19 4.49 20 Bicarbonate as CaCO3 215 mg/L 204 5.05 20 Carbonate as CaCO3 ND 1.00 mg/L ND 20 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document No duplication of this report is allowed,except in its entirety. Page 8 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B215377-No Prep-Wet Chem(Continued) Duplicate(B215377-DUP2) Source:H215202-04 Prepared&Analyzed: 12/21/2021 pH 7.70 pH Units 7.68 0.260 20 Conductivity 297 uS/cm 295 0.676 20 Alkalinity,CaCO3 172 mg/L 169 2.00 20 Hydroxide as CaCO3 ND 1.00 mg/L ND 20 Bicarbonate as CaCO3 172 mg/L 169 2.00 20 Carbonate as CaCO3 ND 1.00 mg/L ND 20 Batch: B215382-No Prep- Wet Chem Blank(B215382-BLK1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica ND 1.00 mg/L Blank(B215382-BLK2) Prepared: 12/21/2021 Analyzed:12/22/2021 Silica ND 1.00 mg/L Blank(B215382-BLK3) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica ND 1.00 mg/L LCS(B215382-BS1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica 5.37 mg/L 4.97 108 90-110 Matrix Spike(B215382-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Silica 23.8 1.00 mg/L 4.97 19.5 86.3 80-120 Matrix Spike Dup(B215382-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Silica 24.2 1.00 mg/L 4.97 19.5 93.0 80-120 1.38 20 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 9 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: 8215382-No Prep- Wet Chem(Continued) Reference(B215382-SRM1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica 32.8 mg/L 33.0 99.2 85-115 Batch: B215383-No Prep- Wet Chem Blank(B215383-BLK1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron ND 0.050 mg/L Blank(B215383-BLK2) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron ND 0.050 mg/L Blank(B215383-BLK3) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.0070 0.050 mg/L LCS(B215383-BS1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.52 mg/L 0.500 103 90-110 Matrix Spike(B215383-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Iron 0.81 0.050 mg/L 0.538 0.17 118 80-120 Matrix Spike Dup(B215383-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Iron 0.78 0.050 mg/L 0.538 0.17 113 80-120 3.78 20 Reference(B215383-SRM1) Prepared: 12/21/2021 Analyzed:12/22/2021 Iron 0.43 mg/L 0.435 98.6 85-115 Batch: 5215384-No Prep- Wet Chem Blank(B215384-BLK1) Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese ND 0.0500 mg/L The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 10 of 17 4 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B215384-No Prep- Wet Chem(Continued) Blank(B215384-BLK2) Prepared: 12/21/2021 Analyzed: 12/22/2021 Manganese ND 0.0500 mg/L Blank(B215384-BLK3) Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.00200 0.0500 mg/L LCS(B215384-BS1) Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.477 mg/L 0.500 95.4 90-110 Matrix Spike(B215384-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.710 0.0500 mg/L 0.564 0.0690 114 80-120 Matrix Spike Dup(B215384-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.726 0.0500 mg/L 0.564 0.0690 116 80-120 2.23 20 Reference(B215384-SRM1) Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 2.00 mg/L 1.92 104 85-115 Batch: B220043-[CALC] Blank(B220043-BLK1) Prepared&Analyzed: 1/4/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 11 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-[CALC](Continued) Blank(B220043-BLK2) Prepared: 1/4/2022 Analyzed: 1/5/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L Blank(B220043-BLK3) Prepared:1/4/2022 Analyzed: 1/5/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L LCS(B220043-BS1) Prepared: 1/4/2022 Analyzed:1/5/2022 Ortho-phosphate 1.02 mg/L Nitrate ND 1.00 mg/L 80-120 Nitrite ND 0.100 mg/L 80-120 Bromide 0.544 mg/L 0.600 90.7 80-120 Chloride 10.9 mg/L 10.0 109 80-120 Fluoride 0.594 mg/L 0.600 99.0 80-120 Sulfate 10.6 mg/L 10.0 106 80-120 Phosphate-P 0.331 mg/L 0.400 82.8 80-120 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 12 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD*** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-[CALCJ(Continued) Duplicate(B220043-DUP1) Source:H215202-02 Prepared&Analyzed: 1/4/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L ND 20 Nitrite ND 0.100 mg/L ND 20 Bromide ND 0.250 mg/L ND 20 Chloride 8.25 5.00 mg/L 8.34 1.18 20 Fluoride 0.111 0.250 mg/L 0.110 0.362 20 Sulfate 2.61 5.00 mg/L 2.62 0.313 20 Phosphate-P ND 0.250 mg/L ND 20 Matrix Spike(B220043-MS1) Source:H215202-03 Prepared&Analyzed:1/4/2022 Ortho-phosphate 1.30 0.766 mg/L Nitrate ND 1.00 mg/L ND 75-125 Nitrite ND 0.100 mg/L ND 75-125 Bromide 0.615 0.250 mg/L 0.576 ND 107 75-125 Chloride 19.8 5.00 mg/L 9.60 8.38 119 75-125 Fluoride 0.831 0.250 mg/L 0.576 0.178 113 75-125 Sulfate 12.6 5.00 mg/L 9.60 1.42 116 75-125 Phosphate-P 0.426 0.250 mg/L 0.384 ND 111 75-125 Reference(B220043-SRM1) Prepared:1/4/2022 Analyzed:1/5/2022 Chloride 56.5 mg/L 57.5 98.3 85-115 Fluoride 3.39 mg/L 3.46 98.0 85-115 Sulfate 87.5 mg/L 87.0 101 85-115 Reference(B220043-SRM2) Prepared:1/4/2022 Analyzed:1/5/2022 Ortho-phosphate 3.97 mg/L Phosphate-P 1.29 mg/L 1.43 90.5 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 13 of 17 ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-No Prep- Wet Chem(Continued) Reference(B220043-SRM3) Prepared: 1/4/2022 Analyzed: 1/5/2022 Bromide 0.776 mg/L 0.839 92.5 85-115 Batch: B220044-[CALCJ Blank(B220044-BLK1) Prepared&Analyzed:1/4/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L Blank(B220044-BLK2) Prepared: 1/4/2022 Analyzed: 1/5/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L Blank(B220044-BLK3) Prepared:1/4/2022 Analyzed: 1/5/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L LCS(B220044-BS1) Prepared:1/4/2022 Analyzed:1/5/2022 Total Hardness 17.4 mg/L Sodium 30.5 mg/L 32.0 95.4 85-115 Magnesium 1.50 mg/L 1.60 94.0 85-115 Calcium 4.49 mg/L 4.00 112 85-115 Potassium 4.56 mg/L 4.00 114 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 14 of 17 C, ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD*** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B220044-[CALCJ(Continued) Duplicate(B220044-DUP1) Source:H215202-02 Prepared&Analyzed: 1/4/2022 Total Hardness 177 7.05 mg/L Sodium 4.91 10.0 mg/L 4.89 0.277 20 Magnesium 1.39 0.500 mg/L 1.39 0.144 20 Calcium 68.3 2.00 mg/L 68.3 0.00805 20 Potassium 0.524 1.00 mg/L 0.519 0.997 20 Matrix Spike(B220044-MS1) Source:H215202-03 Prepared&Analyzed: 1/4/2022 Total Hardness 155 7.05 mg/L Sodium 37.9 10.0 mg/L 30.7 5.09 107 75-125 Magnesium 2.32 0.500 mg/L 1.54 1.03 83.8 75-125 Calcium 58.3 2.00 mg/L 3.84 56.6 45.6 75-125 Potassium 4.83 1.00 mg/L 3.84 0.756 106 75-125 Reference(B220044-SRM1) Prepared:1/4/2022 Analyzed: 1/5/2022 Potassium 12.2 mg/L 12.4 98.3 85-115 -------------------- Reference(B220044-SRM2) Prepared:1/4/2022 Analyzed: 1/5/2022 Total Hardness 261 mg/L Magnesium 36.8 mg/L 38.0 97.0 85-115 Calcium 43.8 mg/L 41.5 106 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 15 of 17 C� ONWASA Hubert WTP Project: Hubert Source Water Red 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Notes and Definitions Item Definition Dry Sample results reported on a dry weight basis. ND Analyte NOT DETECTED at or above the reporting limit. The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 16 of 17 ® 0 CHAIN OF CUSTODY I III I I II II[II oil II NwAsA ONWASA Laboratory 228 Georgetown Road Pagt 1 of 1 H 21 5 2 0 3 Jacksonville,North Carolina 28540 Phone:(910)389-8511 COC Number Fax:(910)455-5607 Lab Work Order Numb' H215203 tilent Name Project Name equested Analyses held Analysis xequestea turn Arouno Hubert WTP Hubert Source Water Red c c Client Contact Project Number o 0 Rush requests subject to additional James Arnold [none] a re charge. Address Project Description 'x 10 374 Hubert Boulevard c o Rush requests subject to lab o v q .6 ' n approval. City PO Number m = p I M onq Hubert State/Zip Shipped B " (9 n y ra ' V, tna Standard)days) NC,28539 °a v' © n; Phone/Fax Tracking Number m o 7.2 cm n •''CU •_* (910)937 7576/ . m u 0 0 p n n Expedited(days) 0 Sampler Sampler Signature r'l cl 3 n m n Plant Personnel oo m o \ o o O Due Date m m r- r- 7 — Preservation Code Sample type Matrix Container Sample Name or Field ID Sampled Date Sampled Time Code Code _ —Count P::A Sample Comments HWTP Raw Red Tap 1 4/4/0/.t/ O?c/ G DW 1 1 HWTP Well#1 12/11/11 On( G RW 1 1 _ HWTP Well#11 1.2/20/aI 0}[3 G RW 1 1 HWTP Well#14 IV:IV i 0 9 ;7 G RW 1 1 HWTP Well#2 12/2d/21 i 1 c b G RW 1 1 HWTP Well#4 1.2/..n/EI II ol:i G RW 1 1 HWTP Well#7 11/20/a 1 a)49 G RW 1 1 g Relinquished By Date/Time Received By Date/Time Gb,,f eri H 1debuf- 41_4.)-ilt 41-.1/-xi / /s4/d uz it t /z/.1/emu4 jj•r,tz Relinquished By Date/Time Received By Date/Time Comments Relinquished By Date/Time Received By Date/Time Cooler Numbers and Temperatures Receive Temp: y°C pH: - Intials: ifi-r.-- Matrix Codes: DW=DW,RW=RW Preserv.Codes: A=Cool 6 degC •Indicates Field Test Analysis Cont.Codes P=P 250 ml ONWASA Laboratory 228 Georgetown Road Jacksonville NC 28540 ONWASA (910) 389-8511 January 12, 2022 James Arnold Hubert WTP 374 Hubert Boulevard Hubert, NC 28539 RE: Hubert Source Water Blue Enclosed are the results of analyses for samples received by our laboratory on 12/21/2021. If you have any questions concerning this report, please feel free to contact me. Sincerely, 14e141.2t. Todd A. Roberts For James Arnold Hubert Water Treatment Plant Supervisor Table of Contents Cover Letter 1 Samples in Report 3 Sample Results 4 Quality Assurance Results 9 Qualifiers and Definitions 17 Chain of Custody PDF 18 r- ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Samples in this Report Lab ID Sample/Location Matrix Date Sampled Date Received H215202-01 HWTP Raw Blue Tap 1 Wells 3,6,8,9,10,12,13,15 DW 12/21/2021 12/21/2021 H215202-02 HWTP Well#10 Hubert Well#10 DW 12/21/2021 12/21/2021 H215202-03 HWTP Well#12 HWTP Well#12 DW 12/21/2021 12/21/2021 H215202-04 HWTP Well#13 Hubert Well#13 DW 12/21/2021 12/21/2021 H215202-05 HWTP Well#15 Hubert Well#15 DW 12/21/2021 12/21/2021 H215202-06 HWTP Well#3 Hubert Well#3 DW 12/21/2021 12/21/2021 H215202-07 HWTP Well#6 Hubert Well#6 DW 12/21/2021 12/21/2021 H215202-08 HWTP Well#8 Hubert Well#8 DW 12/21/2021 12/21/2021 H215202-09 HWTP Well#9 Hubert Well#9 DW 12/21/2021 12/21/2021 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 3 of 18 A. ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results Sample: HWTP Raw Blue Tap 1 H215202-01(DW) Wells 3,6,8,9,10,12,13,15 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/04/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/04/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Chloride 8.83 5.00 mg/L 01/04/2022 DMK EPA 300.1 Fluoride 0.147 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sulfate 2.35 5.00 mg/L 01/04/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sodium 5.54 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.24 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 66.0 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.815 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.17 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0690 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 318 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 189 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/04/2022 DMK EPA 300.1 Silica 19.5 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 170 7.05 mg/L 01/04/2022 DMK Calculated Sample: HWTP Well #10 H215202-02(DW) Hubert Well#10 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/04/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/04/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Chloride 8.34 5.00 mg/L 01/04/2022 DMK EPA 300.1 Fluoride 0.110 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sulfate 2.62 5.00 mg/L 01/04/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sodium 4.89 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.39 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 68.3 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.519 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.43 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0780 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 323 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 193 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/04/2022 DMK EPA 300.1 Silica 18.3 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 177 7.05 mg/L 01/04/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 4 of 18 Cis ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #12 H215202-03(DW) HWTP Well#12 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/04/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/04/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Chloride 8.38 5.00 mg/L 01/04/2022 DMK EPA 300.1 Fluoride 0.178 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sulfate 1.42 5.00 mg/L 01/04/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sodium 5.09 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.03 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 56.6 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.756 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.34 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0640 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 275 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 164 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/04/2022 DMK EPA 300.1 Silica 19.2 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 146 7.05 mg/L 01/04/2022 DMK Calculated Sample: HWTP Well #13 H215202-04(DW) Hubert Well#13 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/04/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/04/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Chloride 8.35 5.00 mg/L 01/04/2022 DMK EPA 300.1 Fluoride 0.0988 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sulfate 2.59 5.00 mg/L 01/04/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sodium 5.00 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.12 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 62.1 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.568 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.77 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0870 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 295 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 169 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/04/2022 DMK EPA 300.1 Silica 14.8 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 160 7.05 mg/L 01/04/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 5 of 18 6i ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #15 H215202-05(DW) Hubert Well#15 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/04/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/04/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/04/2022 DMK EPA 300.1 Chloride 8.78 5.00 mg/L 01/04/2022 DMK EPA 300.1 Fluoride 0.125 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sulfate 1.64 5.00 mg/L 01/04/2022 DMK EPA 300.1 Phosphate-P 0.0930 0.250 mg/L 01/04/2022 DMK EPA 300.1 Sodium 5.33 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.33 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 72.9 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.694 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.32 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0780 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 342 uS/cm 12/21/2021 DMN SM 2510 8 Alkalinity,CaCO3 208 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/04/2022 DMK EPA 300.1 Silica 18.4 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 188 7.05 mg/L 01/04/2022 DMK Calculated Sample: HWTP Well #3 H215202-06(DW) Hubert Well#3 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.86 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.149 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 3.23 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.21 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.23 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 66.9 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.657 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.66 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0660 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 317 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 185 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 16.8 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 172 7.05 mg/L 01/04/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document No duplication of this report is allowed,except in its entirety. Page 6 of 18 ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #6 H215202-07(DW) Hubert Well#6 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 10.1 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.158 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 4.10 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.17 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.14 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 66.3 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.731 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.37 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0730 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 317 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 183 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 18.2 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 170 7.05 mg/L 01/04/2022 DMK Calculated Sample: HWTP Well #8 H215202-08(DW) Hubert Well#8 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 8.45 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.210 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate 2.06 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 5.15 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.12 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 62.8 2.00 mg/L 01/04/2022 DMK EPA 300.1 Potassium 0.776 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.49 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.0680 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 299 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 180 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 17.3 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 162 7.05 mg/L 01/04/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 7 of 18 C� ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Sample Results (Continued) Sample: HWTP Well #9 H215202-09(DW) Hubert Well#9 Reporting Date Analyst Analyte Result Qual Limit Units Analyzed Initials Method Nitrate ND 1.00 mg/L 01/05/2022 DMK EPA 300.1 Nitrite ND 0.100 mg/L 01/05/2022 DMK EPA 300.1 Bromide ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Chloride 9.21 5.00 mg/L 01/05/2022 DMK EPA 300.1 Fluoride 0.145 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sulfate ND 5.00 mg/L 01/05/2022 DMK EPA 300.1 Phosphate-P ND 0.250 mg/L 01/05/2022 DMK EPA 300.1 Sodium 9.31 10.0 mg/L 01/04/2022 DMK EPA 300.1 Magnesium 1.95 0.500 mg/L 01/04/2022 DMK EPA 300.1 Calcium 83.8 2.00 mg/L 01/04/2022 DMK EPA 300.1 ' Potassium 1.99 1.00 mg/L 01/04/2022 DMK EPA 300.1 Iron 0.51 0.050 mg/L 12/22/2021 DMK EPA 149 A Rev 1 Manganese 0.179 0.0500 mg/L 12/22/2021 DMK EPA 164 A Rev 0 Conductivity 408 uS/cm 12/21/2021 DMN SM 2510 B Alkalinity,CaCO3 245 mg/L 12/21/2021 DMN EPA 310.1 Ortho-phosphate ND 0.766 mg/L 01/05/2022 DMK EPA 300.1 Silica 30.5 1.00 mg/L 12/22/2021 DMK EPA 122-A Rev 9 Total Hardness 217 7.05 mg/L 01/04/2022 DMK Calculated The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 8 of 18 ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control *** DEFAULT GENERAL METHOD *** Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B215377-No Prep- Wet Chem Blank(B215377-BLK1) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 10.2 mg/L Conductivity 4.00 uS/cm Blank(B215377-BLK2) Prepared&Analyzed: 12/21/2021 Conductivity 3.00 uS/cm Alkalinity,CaCO3 10.2 mg/L Blank(B215377-BLK3) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 10.3 mg/L Conductivity 3.00 uS/cm LCS(B215377-BS1) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 247 mg/L 250 98.9 90-110 pH 9.76 pH Units 90-110 Conductivity 531 uS/cm 90-110 LCS(B215377-BS2) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 244 mg/L 250 97.4 90-110 Conductivity 488 uS/cm 90-110 pH 9.71 pH Units 90-110 LCS(B215377-BS3) Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 247 mg/L 250 98.9 90-110 Conductivity 487 uS/cm 90-110 pH 9.68 pH Units 90-110 Duplicate(B215377-DUP1) Source:H215203-01 Prepared&Analyzed: 12/21/2021 Alkalinity,CaCO3 215 mg/L 204 5.05 20 Hydroxide as CaCO3 ND 1.00 mg/L ND 20 Conductivity 358 uS/cm 356 0.560 20 pH 7.52 pH Units 7.19 4.49 20 Carbonate as CaCO3 ND 1.00 mg/L ND 20 Bicarbonate as CaCO3 215 mg/L 204 5.05 20 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document No duplication of this report is allowed,except in its entirety. Page 9 of 18 ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B215377-No Prep- Wet Chem(Continued) Duplicate(B215377-DUP2) Source:H215202-04 Prepared&Analyzed: 12/21/2021 Conductivity 297 uS/cm 295 0.676 20 Hydroxide as CaCO3 ND 1.00 mg/L ND 20 Alkalinity,CaCO3 172 mg/L 169 2.00 20 pH 7.70 pH Units 7.68 0.260 20 Carbonate as CaCO3 ND 1.00 mg/L ND 20 Bicarbonate as CaCO3 172 mg/L 169 2.00 20 Batch: B215382-No Prep- Wet Chem Blank(B215382-BLK1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica ND 1.00 mg/L Blank(B215382-BLK2) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica ND 1.00 mg/L Blank(B215382-BLK3) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica ND 1.00 mg/L LCS(B215382-BS1) Prepared: 12/21/2021 Analyzed:12/22/2021 Silica 5.37 mg/L 4.97 108 90-110 Matrix Spike(B215382-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Silica 23.8 1.00 mg/L 4.97 19.5 86.3 80-120 Matrix Spike Dup(B215382-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Silica 24.2 1.00 mg/L 4.97 19.5 93.0 80-120 1.38 20 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 10 of 18 ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B215382-No Prep- Wet Chem(Continued) Reference(B215382-SRM1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Silica 32.8 mg/L 33.0 99.2 85-115 Batch: B215383-No Prep- Wet Chem Blank(B215383-BLK1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron ND 0.050 mg/L Blank(B215383-BLK2) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron ND 0.050 mg/L Blank(B215383-BLK3) Prepared: 12/21/2021 Analyzed:12/22/2021 Iron 0.0070 0.050 mg/L LCS(B215383-BS1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.52 mg/L 0.500 103 90-110 Matrix Spike(B215383-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.81 0.050 mg/L 0.538 0.17 118 80-120 Matrix Spike Dup(8215383-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.78 0.050 mg/L 0.538 0.17 113 80-120 3.78 20 Reference(B215383-SRM1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Iron 0.43 mg/L 0.435 98.6 85-115 Batch: 8215384-No Prep- Wet Chem Blank(B215384-BLK1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Manganese ND 0.0500 mg/L The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 11 of 18 C. ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B215384-No Prep- Wet Chem(Continued) Blank(B215384-BLK2) Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese ND 0.0500 mg/L Blank(B215384-BLK3) Prepared:12/21/2021 Analyzed: 12/22/2021 Manganese 0.00200 0.0500 mg/L LCS(B215384-BS1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Manganese 0.477 mg/L 0.500 95.4 90-110 Matrix Spike(B215384-MS1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.710 0.0500 mg/L 0.564 0.0690 114 80-120 Matrix Spike Dup(B215384-MSD1) Source:H215202-01 Prepared: 12/21/2021 Analyzed:12/22/2021 Manganese 0.726 0.0500 mg/L 0.564 0.0690 116 80-120 2.23 20 Reference(B215384-SRM1) Prepared: 12/21/2021 Analyzed: 12/22/2021 Manganese 2.00 mg/L 1.92 104 85-115 Batch: B220043-[CALCJ Blank(B220043-BLK1) Prepared&Analyzed: 1/4/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 12 of 18 A. ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD *** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-[CALC](Continued) Blank(B220043-BLK2) Prepared: 1/4/2022 Analyzed: 1/5/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L Blank(B220043-BLK3) Prepared: 1/4/2022 Analyzed:1/5/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L Nitrite ND 0.100 mg/L Bromide ND 0.250 mg/L Chloride ND 5.00 mg/L Fluoride ND 0.250 mg/L Sulfate ND 5.00 mg/L Phosphate-P ND 0.250 mg/L LCS(B220043-BS1) Prepared:1/4/2022 Analyzed:1/5/2022 Ortho-phosphate 1.02 mg/L Nitrate ND 1.00 mg/L 80-120 Nitrite ND 0.100 mg/L 80-120 Bromide 0.544 mg/L 0.600 90.7 80-120 Chloride 10.9 mg/L 10.0 109 80-120 Fluoride 0.594 mg/L 0.600 99.0 80-120 Sulfate 10.6 mg/L 10.0 106 80-120 Phosphate-P 0.331 mg/L 0.400 82.8 80-120 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 13 of 18 • ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD*** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-[CALCJ(Continued) Duplicate(B220043-DUP1) Source:H215202-02 Prepared&Analyzed:1/4/2022 Ortho-phosphate ND 0.766 mg/L Nitrate ND 1.00 mg/L ND 20 Nitrite ND 0.100 mg/L ND 20 Bromide ND 0.250 mg/L ND 20 Chloride 8.25 5.00 mg/L 8.34 1.18 20 Fluoride 0.111 0.250 mg/L 0.110 0.362 20 Sulfate 2.61 5.00 mg/L 2.62 0.313 20 Phosphate-P ND 0.250 mg/L ND 20 Matrix Spike(B220043-MS1) Source:H215202-03 Prepared&Analyzed:1/4/2022 Ortho-phosphate 1.30 0.766 mg/L Nitrate ND 1.00 mg/L ND 75-125 Nitrite ND 0.100 mg/L ND 75-125 Bromide 0.615 0.250 mg/L 0.576 ND 107 75-125 Chloride 19.8 5.00 mg/L 9.60 8.38 119 75-125 Fluoride 0.831 0.250 mg/L 0.576 0.178 113 75-125 Sulfate 12.6 5.00 mg/L 9.60 1.42 116 75-125 Phosphate-P 0.426 0.250 mg/L 0.384 ND 111 75-125 Reference(B220043-SRM1) Prepared:1/4/2022 Analyzed: 1/5/2022 Chloride 56.5 mg/L 57.5 98.3 85-115 Fluoride 3.39 mg/L 3.46 98.0 85-115 Sulfate 87.5 mg/L 87.0 101 85-115 Reference(B220043-SRM2) Prepared:1/4/2022 Analyzed:1/5/2022 Ortho-phosphate 3.97 mg/L Phosphate-P 1.29 mg/L 1.43 90.5 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 14 of 18 A. ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD*** (Continued) Reporting Spike Source %REC RPD Analyte Result Qual Limit Units Level Result %REC Limits RPD Limit Batch: B220043-No Prep- Wet Chem(Continued) Reference(B220043-SRM3) Prepared: 1/4/2022 Analyzed:1/5/2022 Bromide 0.776 mg/L 0.839 92.5 85-115 Batch: B220044-[CALCJ Blank(B220044-BLK1) Prepared&Analyzed: 1/4/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L Blank(B220044-BLK2) Prepared: 1/4/2022 Analyzed:1/5/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L Blank(B220044-BLK3) Prepared:1/4/2022 Analyzed: 1/5/2022 Total Hardness ND 7.05 mg/L Sodium ND 10.0 mg/L Magnesium ND 0.500 mg/L Calcium ND 2.00 mg/L Potassium ND 1.00 mg/L LCS(B220044-BS1) Prepared: 1/4/2022 Analyzed:1/5/2022 Total Hardness 17.4 mg/L Sodium 30.5 mg/L 32.0 95.4 85-115 1 Magnesium 1.50 mg/L 1.60 94.0 85-115 Calcium 4.49 mg/L 4.00 112 85-115 Potassium 4.56 mg/L 4.00 114 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 15 of 18 44 ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Quality Control (Continued) *** DEFAULT GENERAL METHOD*** (Continued) Reporting Spike Source %REC RPD Analyte ResultQual Limit Units Level Result %REC Limits RPD Limit Batch: B220044-[CALCJ(Continued) Duplicate(B220044-DUP1) Source:H215202-02 Prepared&Analyzed: 1/4/2022 Total Hardness 177 7.05 mg/L Sodium 4.91 10.0 mg/L 4.89 0.277 20 Magnesium 1.39 0.500 mg/L 1.39 0.144 20 Calcium 68.3 2.00 mg/L 68.3 0.00805 20 Potassium 0.524 1.00 mg/L 0.519 0.997 20 Matrix Spike(B220044-MS1) Source:H215202-03 Prepared&Analyzed:1/4/2022 Total Hardness 155 7.05 mg/L Sodium 37.9 10.0 mg/L 30.7 5.09 107 75-125 Magnesium 2.32 0.500 mg/L 1.54 1.03 83.8 75-125 Calcium 58.3 2.00 mg/L 3.84 56.6 45.6 75-125 Potassium 4.83 1.00 mg/L 3.84 0.756 106 75-125 Reference(B220044-SRM1) Prepared: 1/4/2022 Analyzed:1/5/2022 Potassium 12.2 mg/L 12.4 98.3 85-115 Reference(B220044-SRM2) Prepared: 1/4/2022 Analyzed:1/5/2022 Total Hardness 261 mg/L Magnesium 36.8 mg/L 38.0 97.0 85-115 Calcium 43.8 mg/L 41.5 106 85-115 The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 16 of 18 Li ONWASA Hubert WTP Project: Hubert Source Water Blue 374 Hubert Boulevard Project Number: Reported: Hubert,NC 28539 Project Manager: James Arnold 01/12/2022 08:42 Notes and Definitions Item Definition Dry Sample results reported on a dry weight basis. ND Analyte NOT DETECTED at or above the reporting limit. The contents of this report apply to the sample(s)analyzed in accordance with the chain of custody document. No duplication of this report is allowed,except in its entirety. Page 17 of 18 CHAIN OF CUSTODY III 1111111121011121 11111 II 41,1 oNwAsA ONWASA Laboratory 228 Georgetown Road Pag( 1 of 1 H 2 1 5 2 0 2 �� Jacksonville,North Carolina 28540 Phone:(910)389-8511 COC Number Fax:(910)455-5607 Lab Work Order Numb( H215202 tiient Name Project Name Requested Analyses tmid Analysis eequesreo turn Arouno Hubert WTP Hubert Source Water Blue c c Client Contact Project Number .2 o Rush requests subject to additional James Arnold [none] u ro charge. Address Project Description r n x v 374 Hubert Boulevard 19 o Ruth requests subject to lab c a- 0 0 0 O CI' approval. City PO Number 1" O = Hubert ar C C- N State/Zip Shipped By •). 0- U, 3 n co to Oct Standard(days) NC,28539 Cu 13 O 0 °; Phone/Fax Tracking Number `CO o oq n " '* • 0'" - (I) O o O Expedited(days) (910)937-7576/ m ? ro ro PaSampler Sampler Signature 0 d 3 at R R Due Date Plant Personnel m u, i � z = Preservation Code Sample Type Matrix Container Sample Name or Field ID Sampled Date Sampled Time Code Code Count P::A Sample Comments HWTP Raw Blue Tap 1 a•.2/-.'tl 0'7K4' G DW 1 1 HWTP Well#10 /J•2I.11 , /050 G RW 1 1 HWTP Well#12 1/2011-.LI fOO to G RW 1 1 HWTP Well#13 /A--AI-r1l C45.2. G RW 1 1 HWTP Well#15 42-1-/-01l /04/ _ G RW 1 1 HWTP Well#3 j.t-li-2/ /ply G RW 1 1 HWTP Well#6 /2- 2/-2./ /O i7 G RW 1 1 — HWTP Well#8 /-j-,t/-1( 0 9Se G RW 1 1 HWTP Well#9 -- _ Relinquished By Date/Time Received By Date/Time C>h.lan A & be ✓ ,c ,, /tit GclJ /J-.2,•d I //Via ' --,fr e 4-a44..44 l7,/L/,/ac:a./ igi% Relinquished By Date/Time Received By Date/Time Comments Relinquished By Date/Time Received By Date/Time Cooler Numbers and Temperatures Receive Temp: °C pH: Intials: Matrix Codes: DW=OW,RW=RW Preserv.Codes: A=Cool 6 degC °Indicates Field Test Analysis Cont.Codes P=P 250 ml APPENDIX C SAFETY DATA SHEET 0 Compass POTASSIUM PERMANGANATE Remediation Chemicals Revision date 4/10/2017 1. PRODUCT AND COMPANY IDENTIFICATION 1.1 Product identifiers Product name: Potassium permanganate Description: minimum as KMn04 1.2 Relevant identified uses of the substance or mixture and uses advised against Identified uses: Chemical oxidation of organic compounds for remediation 1.3 Details of the supplier of the safety data sheet Company Compass Remediation Chemicals 2028 East Ben White Blvd #240-1974 Austin, TX 78741 Telephone (866) 221-9167 1.4 Emergency telephone number Emergency Phone #: CHEMTREC 1-800-424-9300 2. HAZARDS IDENTIFICATION 2.1 Classification of the substance or mixture GHS Classification in accordance with 29 CFR 1910 (OSHA HCS) Oxidizing liquids (Category 2), H272 Acute toxicity, Oral (Category 4), H302 Skin corrosion (Category 1B), H314 Serious eye damage (Category 1), H318 Specific target organ toxicity, single exposure (Category 1, Respiratory System) Specific target organ toxicity, repeated exposure (Category 1, Respiratory System, Central Nervous System) Acute aquatic toxicity (Category 1), H400 Chronic aquatic toxicity (Category 1), H410 For the full text of the H-Statements mentioned in this Section, see Section 16. 2.2 GHS Label elements, including precautionary statements ot,2 Pictogram Signal word Danger Potassium Permanganate Page 1 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Hazard statement(s) H272 May intensify fire; oxidizer. H302 Harmful if swallowed. H314 Causes severe skin burns and eye damage. H370 Causes damage to organs (Respiratory System) H372 Causes damage to organs (Respiratory System, Central Nervous System) through prolonged or repeated exposure H410 Very toxic to aquatic life with long lasting effects. Precautionary statement(s) P210 Keep away from heat. P220 Keep/store away from clothing/combustible materials. P221 Take any precaution to avoid mixing with combustibles. P260 Do not breathe dust P264 Wash skin thoroughly after handling. P270 Do not eat, drink or smoke when using this product. P273 Avoid release to the environment. P280 Wear protective gloves/protective clothing/eye protection/face protection P301 + P312 IF SWALLOWED: Call a POISON CENTER or doctor/ physician if you feel unwell. P301 + P330 + P331 IF SWALLOWED: Rinse mouth. Do NOT induce vomiting. P303 + P361 + P353 IF ON SKIN (or hair): Remove/Take off immediately all Contaminated clothing. Rinse skin with water/ shower. P304 + P340 IF INHALED: Remove victim to fresh air and keep at rest in a position comfortable for breathing. P305 + P351 + P338 IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. P310 Immediately call a POISON CENTER or doctor/ physician. P321 Specific treatment (see supplemental first aid instructions on this label). P363 Wash contaminated clothing before reuse. P370 + P378 In case of fire: Use water for extinction. P391 Collect spillage. P405 Store locked up. P501 Dispose of contents/container in accordance with local/regional/national/international regulations. 2.3 Hazards not otherwise classified (HNOC) or not covered by GHS— none Potassium Permanganate Page 2 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE 3. COMPOSITION/INFORMATION ON INGREDIENTS Substances Chemical name CAS number Sodium Permanganate 7722-64-7 > 97.5 Composition comments All concentrations are in percent by weight unless ingredient is a gas. Gas concentrations are in percent by volume. 4. FIRST AID MEASURES 4.1 Description of first aid measures Inhalation Remove victim to fresh air and keep at rest in a position comfortable for breathing. For breathing difficulties, oxygen may be necessary. Get medical attention immediately. Skin contact Take off immediately all contaminated clothing. Immediately flush skin with plenty of water. Get medical attention immediately. Wash contaminated clothing before reuse. Contact with skin may leave a brown stain of insoluble manganese dioxide. This can be easily removed by washing with a mixture of equal volume of household vinegar and 3% hydrogen peroxide, followed by washing with soap and water. Eye contact Immediately flush with plenty of water for up to 15 minutes. Remove any contact lenses and open eyelids wide apart. Continue rinsing. Get medical attention immediately. Ingestion Immediately rinse mouth and drink plenty of water. Never give anything by mouth to a victim who is unconscious or is having convulsions. Do not induce vomiting. If vomiting occurs, keep head low so that stomach content doesn't get into the lungs. Get medical attention immediately. 4.2 Most important symptoms/effects, acute and delayed Contact with this material will cause burns to the skin, eyes and mucous membranes. Permanent eye damage including blindness could result. 4.3 Indication of immediate medical attention and special treatment needed Provide general supportive measures and treat symptomatically. In case of shortness of breath, give oxygen. Decomposition products are alkaline. Brown stain is insoluble manganese dioxide. Potassium Permanganate Page 3 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE General information In the case of accident or if you feel unwell, seek medical advice immediately (show the label where possible). Ensure that medical personnel are aware of the material(s) involved, and take precautions to protect themselves. Show this safety data sheet to the doctor in attendance. For personal protection, see Section 8 of the SDS. Wash contaminated clothing before reuse. 5. FIREFIGHTING MEASURES 5.1 Suitable extinguishing media Flood with water from a distance, water spray or fog. Unsuitable extinguishing media The following extinguishing media are ineffective: Dry chemical. Foam. Carbon dioxide (CO2). Halogenated materials. 5.2 Specific hazards arising from the chemical May intensify fire; oxidizer. May ignite combustibles (wood, paper, oil, clothing, etc.). Contact with incompatible materials or heat (135 °C/ 275 °F) could result in violent exothermic chemical reaction. Oxidizing agent, may cause spontaneous ignition of combustible materials. By heating and fire, corrosive vapors/gases may be formed. 5.3 Special protective equipment and precautions for firefighters Self-contained breathing apparatus and full protective clothing must be worn in case of fire. Selection of respiratory protection for firefighting: follow the general fire precautions indicated in the workplace. Fire-fighting equipment/instructions Move container from fire area if it can be done without risk. Cool containers exposed to flames with water until well after the fire is out. Prevent runoff from fire control or dilution from entering streams, sewers, or drinking water supply. Dike fire control water for later disposal. Water runoff can cause environmental damage. General fire hazards The product is not flammable. May intensify fire; oxidizer. May ignite combustibles (wood, paper, oil, clothing, etc.). Contact with incompatible materials or heat (135 °C/ 275 °F) could result in violent exothermic chemical reaction. 6. ACCIDENTAL RELEASE MEASURES 6.1 Personal precautions, protective equipment and emergency procedures Keep unnecessary personnel away. Keep upwind. Do not touch damaged containers or spilled material unless wearing appropriate protective clothing. Avoid inhalation of Potassium Permanganate Page 4 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE vapors and contact with skin and eyes. Wear protective clothing as described in Section 8 of this safety data sheet. Local authorities should be advised if significant spillages cannot be contained 6.2 Environmental precautions Prevent further leakage or spillage if safe to do so. Do not let product enter drains. Discharge into the environment must be avoided. 6.3 Methods and materials for containment and cleaning up Keep combustibles (wood, paper, oil, etc.) away from spilled material. Should not be released into the environment. This product is miscible in water. Stop leak if possible without any risk. Dike the spilled material, where this is possible. Clean up spills immediately by sweeping or shoveling up the material. Do not return spilled material to the original container; transfer to a clean metal or plastic drum. To clean up potassium permanganate solutions, follow either of the following two options: Option # 1: Dilute to approximately 6% with water, and then reduce with sodium thiosulfate, a bisulfite or ferrous salt solution. The bisulfite or ferrous salt may require some dilute sulfuric acid (10% w/w) to promote reduction. Neutralize with sodium carbonate to neutral pH, if acid was used. Decant or filter and deposit sludge in approved landfill. Where permitted, the sludge may be drained into sewer with large quantities of water. Option # 2: Absorb with inert media like diatomaceous earth or inert floor dry, collect into a drum and dispose of properly. Do not use saw dust or other incompatible media. Disposal of all materials shall be in full and strict compliance with all federal, state, and local regulations pertaining to permanganates. To clean contaminated floors, flush with abundant quantities of water into sewer, if permitted by federal, state, and local regulations. If not, collect water and treat as described above. 6.4 Reference to other sections For disposal see section 13. 7. HANDLING AND STORAGE 7.1 Precautions for safe handling Take any precaution to avoid mixing with combustibles. Do not get this material in your eyes, on your skin, or on your clothing. Do not breathe dust or mist or vapor of the solution. Use personal protective equipment as recommended in Section 8 of the SDS. If clothing becomes contaminated, remove and wash off immediately. Spontaneous ignition may occur in contact with cloth or paper. When using, do not eat, drink or SDS Potassium Permanganate Page 5 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE smoke. Good personal hygiene is necessary. Wash hands and contaminated areas with water and soap before leaving the work site. Avoid release to the environment. 7.2 Conditions for safe storage, including any incompatibilities Store locked up. Keep container tightly closed and in a well-ventilated place. Store in a cool, dry place. Store away from incompatible materials (See Section 10). Store in accordance with NFPA 430 requirements for Class II oxidizers. 8. EXPOSURE CONTROLS/PERSONAL PROTECTION 8.1 Control parameters Occupational exposure limits US. OSHA Table Z-1 Limits for Air Contaminants (29 CFR 1910.1000) Components Type Value Potassium Permanganate Ceiling 5 mg/m3 (CAS 7722-64-7) US. ACGIH Threshold Limit Values Components Type Value Form Potassium Permanganate TWA 0.1 mg/m3 Inhalable fraction. (CAS 7722-64-7) 0.02 mg/m3 Respirable fraction. US. NIOSH: Pocket Guide to Chemical Hazards Components Type Value Form Potassium Permanganate STEL 3 mg/m3 Fume. (CAS 7722-64-7) TWA 1 mg/m3 Fume. Biological limit values No biological exposure limits noted for the ingredient(s). Exposure guidelines Follow standard monitoring procedures. 8.2 Exposure controls Appropriate engineering controls Provide adequate general and local exhaust ventilation. An eye wash and safety shower must be available in the immediate work area. Personal protective equipment Eye/face protection Wear safety glasses with side shields (or goggles). Wear face shield if there is risk of splashes. Potassium Permanganate Page 6 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Skin protection Hand protection Wear chemical-resistant, impervious gloves. Use protective gloves made of: Rubber or plastic. Suitable gloves can be recommended by the glove supplier. Other Wear appropriate chemical resistant clothing. Rubber or plastic apron. Respiratory protection In case of inadequate ventilation or risk of inhalation of dust, use suitable respiratory equipment with particle filter. In the United States of America, if respirators are used, a program should be instituted to assure compliance with OSHA 29 CFR 1910.134. Measurement Element: Manganese (Mn) 10 mg/m3 Any particulate respirator equipped with an N95, R95, or P95 filter (including N95, R95, and P95 filtering face pieces) except quarter-mask respirators. The following filters may also be used: N99, R99, P99, N100, R100 or P100. Any supplied-air respirator. 25 mg/m3 Any supplied-air respirator operated in a continuous-flow mode. Any powered, air-purifying respirator with a high-efficiency particulate filter. 50 mg/m3 Any air-purifying, full-face piece respirator equipped with an N100, R100, or P100 filter. Any supplied-air respirator with a tight-fitting face piece that is operated in a continuous-flow mode. Respiratory protection cont. Any powered, air-purifying respirator with a tight-fitting face piece and a high-efficiency particulate filter. Any self-contained breathing apparatus with a full face piece. Any supplied-air respirator with a full face piece. 500 mg/m3 Any supplied-air respirator operated in a pressure-demand or other positive-pressure mode. SDS Potassium Permanganate Page 7 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Emergency or planned entry into unknown concentrations or IDLH conditions - Any self-contained breathing apparatus that has a full face piece and is operated in a pressure-demand or other positive-pressure mode. Escape Any air-purifying, full-face piece respirator equipped with an N100, R100, or P100 filter. Any appropriate escape- type, self-contained breathing apparatus. Thermal hazards Wear appropriate thermal protective clothing, when necessary. General hygiene Considerations When using, do not eat, drink or smoke. Keep from contact with clothing and other combustible materials. Remove and wash contaminated clothing promptly. Wash hands before breaks and immediately after handling the product. Handle in accordance with good industrial hygiene and safety practice. 9. PHYSICAL AND CHEMICAL PROPERTIES 9.1 Information on basic physical and chemical properties a) Appearance Form: Dark purple solid with metallic luster. b) Odor Odorless c) Odor Threshold No data available d) pH Not applicable e) Melting point/freezing point Starts to decompose with evolution of oxygen (02) at temperatures above 150 °C. Once initiated, the decomposition is exothermic and self-sustaining. f) Initial boiling point and boiling range Not applicable g) Flash point Not applicable h) Evaporation rate Not applicable i) Flammability (solid, gas) Non flammable j) Upper/lower flammability or explosive limits Not applicable k) Vapor pressure < 0 kPa at 25°C I) Vapor density Not applicable m) Relative density 2.7 (20 °C) ( Water = 1) n) Water solubility 6 % (20 °C) o) Partition coefficient: n-octanol/water No data available p) Auto-ignition temperature No data available Potassium Permanganate Page 8 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE q) Decomposition temperature 464 °F (240 °C) r) Viscosity No data available Other Information Density 2.70 g/cm3 Explosive properties Not explosive. Can explode in contact with sulfuric acid, peroxides, and metal powders. Molecular formula H-Mn-04.K Molecular weight 158.03 g/mol 158.03 Oxidizing properties Strong oxidizing agent. 10. STABILITY AND REACTIVITY 10.1 Reactivity The product is stable and non-reactive under normal conditions of use, storage and transport. 10.2 Chemical stability Stable at normal conditions. 10.3 Possibility of hazardous reactions Contact with combustible material may cause fire. Can explode in contact with sulfuric acid, peroxides and metal powders. Starts to decompose with evolution of oxygen (02) at temperatures above 150 °C. Once initiated, the decomposition is exothermic and self- sustaining. 10.4 Conditions to avoid Contact with incompatible materials or heat (135 °C/ 275 °F) could result in violent exothermic chemical reaction. 10.5 Incompatible materials Acids. Peroxides. Reducing agents. Combustible material. Metal powders. Contact with hydrochloric acid liberates chlorine gas. 10.6 Hazardous decomposition products By heating and fire, corrosive vapors/gases may be formed. 11. TOXICOLOGICAL INFORMATION 11.1 Information on toxicological effects Information on likely routes of exposure Ingestion Harmful if swallowed. Inhalation May cause irritation to the respiratory system. SDS Potassium Permanganate Page 9 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Skin contact Causes severe skin burns. Eye contact Causes serious eye damage. Symptoms related to the physical, chemical and toxicological characteristics Contact with this material will cause burns to the skin, eyes and mucous membranes. Permanent eye damage including blindness could result. Information on toxicological effects Acute toxicity Harmful if swallowed. Components Species Test Results Potassium permanganate (CAS 7722-64-7) Acute Dermal LD50 Rat 2000 mg/kg Oral LD50 Rat 2000 mg/kg Skin corrosion/irritation Causes severe skin burns. Serious eye damage/eye irritation Causes serious eye damage Respiratory or skin sensitization Respiratory sensitization Not classified. Skin sensitization Not classified. Germ cell mutagenicity Not classified. Carcinogenicity Not classified. Reproductive toxicity Not classified. Specific target organ toxicity - single exposure Causes damage to organs (respiratory system). Specific target organ toxicity - repeated exposure Causes damage to organs (respiratory system, central nervous system) through prolonged or repeated exposure. Aspiration hazard Not classified. Chronic effects May cause damage to respiratory system. Prolonged exposure, usually over many years, to manganese oxide fume/dust can lead to chronic manganese poisoning, chiefly affecting the central nervous system. Chronic effects Chronic effects are not expected when this product is used as intended. SDS Potassium Permanganate Page 10 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE 12. ECOLOGICAL INFORMATION 12.1 Toxicity Very toxic to aquatic life with long lasting effects. 12.2 Persistence and degradability Expected to be readily converted by oxidizable materials to insoluble manganese oxide. 12.3 Bioaccumulative potential Potential to bioaccumulate is low. so il Mobility in so I The product is miscible with water. May spread in water systems. 12.5 Results of PBT and vPvB assessment PBT/vPvB assessment not available as chemical safety assessment not required/not conducted 12.6 Other adverse effects None known. 13. DISPOSAL CONSIDERATIONS Disposal instructions Dispose of contents/container in accordance with local/regional/national/international regulations. Hazardous waste code D001: Ignitable waste The Waste code should be assigned in discussion between the user, the producer and the waste disposal company. Waste from residues/ Unused products Do not allow this material to drain into sewers/water supplies. Contaminated packaging Since emptied containers may retain product residue, follow label warnings even after container is emptied. Rinse container at least three times to an absence of pink color before disposing. Empty containers should be taken to an approved waste handling site for recycling or disposal. 14. TRANSPORT INFORMATION DOT (US) UN number: 1490 Class: 5.1 Packing group: II Proper shipping name: Potassium permanganate Potassium Permanganate Page 11 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Special precautions for user Read safety instructions, SDS and emergency procedures before handling. Special provisions IB8, IP2, IP4, T3, TP33 Packaging exceptions 152 Packaging non bulk 212 Packaging bulk 240 IATA UN number UN1490 UN proper shipping name Potassium permanganate Transport hazard class(es) Class 5.1 Subsidiary risk - Label(s) 5.1 Packing group II Environmental hazards Yes ERG Code 5L Special precautions for user Read safety instructions, SDS and emergency procedures before handling. IMDG UN number UN1490 UN proper shipping name Potassium permanganate Transport hazard class(es) Class 5.1 Subsidiary risk - Label(s) 5.1 Packing group II Environmental hazards Marine pollutant Yes EmS F-H, S-Q Special precautions for user Read safety instructions, SDS and emergency procedures before handling. Transport in bulk according to Annex II of MARPOL 73/78 and the IBC Code Not applicable Potassium Permanganate Page 12 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE 15. REGULATORY INFORMATION US federal regulations This product is a "Hazardous Chemical" as defined by the OSHA Hazard Communication Standard, 29 CFR 1910.1200. All components are on the U.S. EPA TSCA InventoryLis t. Drug Enforcement Administration (DEA) (21 CFR 1310.02 (b) 8: List II chemical. Department of Homeland Security (DHS) Chemical Facility Anti-Terrorism Standards (6 CFR 27, Appendix A): Listed. TSCA Section 12(b) Export Notification (40 CFR 707, Subpt. D) Not regulated. US. OSHA Specifically Regulated Substances (29 CFR 1910.1001-1050) Not listed. CERCLA Hazardous Substance List (40 CFR 302.4) Potassium permanganate (CAS 7722-64-7) LISTED Superfund Amendments and Reauthorization Act of 1986 (SARA) Hazard categories Immediate Hazard - Yes Delayed Hazard - Yes Fire Hazard —Yes Pressure Hazard - No Reactivity Hazard - No SARA 302 Extremely hazardous substance Not listed. SARA 311/312 Hazardous chemical Yes SARA 313 (TRI reporting) Chemical name CAS number % by wt. Potassium Permanganate 7722-64-7 > 97.5 Other federal regulations Clean Air Act (CAA) Section 112 Hazardous Air Pollutants (HAPs) List Potassium permanganate (CAS 7722-64-7) Clean Air Act (CAA) Section 112(r) Accidental Release Prevention (40 CFR 68.130) Not regulated. Safe Drinking Water Act (SDWA) Not regulated. Potassium Permanganate Page 13 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE Drug Enforcement Administration (DEA). List 2, Essential Chemicals (21 CFR 1310.02(b) and 1310.04(f)(2) and Chemical Code Number Potassium permanganate (CAS 7722-64-7) 6579 Drug Enforcement Administration (DEA). List 1 & 2 Exempt Chemical Mixtures (21 CFR 1310.12(c)) Potassium permanganate (CAS 7722-64-7) 15 % wt DEA Exempt Chemical Mixtures Code Number Potassium permanganate (CAS 7722-64-7) 6579 US state regulations This product does not contain a chemical known to the State of California to cause cancer, birth defects or other reproductive harm. California OSH Hazardous Substance List: Listed. US. Massachusetts RTK - Substance List Potassium permanganate (CAS 7722-64-7) US. New Jersey Worker and Community Right-to-Know Act Potassium permanganate (CAS 7722-64-7) US. Pennsylvania Worker and Community Right-to-Know Law Potassium permanganate (CAS 7722-64-7) US. Rhode Island RTK Potassium permanganate (CAS 7722-64-7) US. California Proposition 65 US - California Proposition 65 - Carcinogens & Reproductive Toxicity (CRT): Listed substance Not listed. 16. OTHER INFORMATION Full text of H-Statements referred to under sections 2 and 3. Acute Tox. Acute toxicity Aquatic Acute Acute aquatic toxicity Aquatic Chronic Chronic aquatic toxicity Eye Dam. Serious eye damage H272 May intensify fire; oxidizer. H302 Harmful if swallowed. H314 Causes severe skin burns and eye damage. H318 Causes serious eye damage. H400 Very toxic to aquatic life. H410 Very toxic to aquatic life with long lasting effects. Ox. Sol. Oxidizing solids Skin Corr. Skin corrosion SDS Potassium Permanganate Page 14 of 15 SAFETY DATA SHEET - POTASSIUM PERMANGANATE NFPA Rating 410 OX List of abbreviations GHS: Globally Harmonized System of Classification and Labeling of hazardous properties of Chemicals. TWA: Time weighted average. LD50: Lethal Dose, 50%. LC50: Lethal Concentration, 50%. IMDG: International Maritime Dangerous Goods. IATA: International Air Transport Association. MARPOL: International Convention for the Prevention of Pollution from Ships. Disclaimer The information contained herein is accurate to the best of our knowledge. However, data, safety standards and government regulations are subject to change and, therefore, holders and users should satisfy themselves that they are aware of all current data and regulations relevant to their particular use of product. COMPASS REMEDIATION CHEMICALS DISCLAIMS ALL LIABILITY FOR RELIANCE ON THE COMPLETENESS OR ACCURACY OR THE INFORMATION INCLUDED HEREIN. COMPASS REMEDIATION CHEMICALS MAKES NO WARRANTY, EITHER EXPRESS OR IMPLIED, INCLUDING, BUT NOT LIMITED TO, ANY WARRANTIES OF MERCHANTIABILITY OR FITNESS FOR PARTICULAR USE OR PURPOSE OF THE PRODUCT DESCRIBED HEREIN. All conditions relating to storage, handling, and use of the product are beyond the control of Compass Remediation Chemicals and shall be the sole responsibility of the holder or user of the product. SDS Potassium Permanganate Page 15 of 15 AMEROCHEM CORPORATION SAFETY DATA SHEET 1. Identification Product identifier AOC 789(PERMANGANTE STAIN CLEANER) Other means of identification None. Recommended use ALL PROPER AND LEGAL PURPOSES Recommended restrictions None known. Manufacturer/Importer/Supplier/Distributor information Manufacturer Company name Amerochem Corporation. Address 1885 Old Airport Road New Bern,NC 28562 Telephone 1-800-990-4949 E-mail Not available. Emergency phone number 800-424-9300 CHEMTREC 2. Hazard(s) identification Physical hazards Not classified. Health hazards Serious eye damage/eye irritation Category 1 Environmental hazards Not classified, OSHA defined hazards Not classified. Label elements Pf Signal word Danger Hazard statement Causes serious eye damage. Precautionary statement Prevention Wear eye protection/face protection. Response If in eyes: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. Immediately call a poison center/doctor. Storage Store away from incompatible materials. Disposal Dispose of waste and residues in accordance with local authority requirements. Hazard(s)not otherwise None known. classified(HNOC) Supplemental information None. 3. Composition/information on ingredients Mixtures Chemical name Common name and synonyms CAS number 11/0 ACETIC ACID 64-19-7 4.95 Other components below reportable levels 95.05 *Designates that a specific chemical identity and/or percentage of composition has been withheld as a trade secret. 4. First-aid measures Inhalation Move to fresh air. Call a physician if symptoms develop or persist. Skin contact Wash off with soap and water. Get medical attention if irritation develops and persists. Eye contact Immediately flush eyes with plenty of water for at least 15 minutes. Remove contact lenses, if present and easy to do. Continue rinsing. Get medical attention immediately. SIDS US 1 /7 Ingestion Rinse mouth. Get medical attention if symptoms occur. Most important Severe eye irritation. Symptoms may include stinging, tearing,redness,swelling,and blurred symptoms/effects,acute and vision. Permanent eye damage including blindness could result. delayed Indication of immediate Provide general supportive measures and treat symptomatically. Keep victim under observation. medical attention and special Symptoms may be delayed. treatment needed General information Ensure that medical personnel are aware of the material(s)involved,and take precautions to protect themselves. 5. Fire-fighting measures Suitable extinguishing media Water fog. Foam. Dry chemical powder. Carbon dioxide (CO2). Unsuitable extinguishing Do not use water jet as an extinguisher,as this will spread the fire. media Specific hazards arising from During fire,gases hazardous to health may be formed. the chemical Special protective equipment Self-contained breathing apparatus and full protective clothing must be worn in case of fire. and precautions for firefighters Fire fighting Move containers from fire area if you can do so without risk. equipment/instructions Specific methods Use standard firefighting procedures and consider the hazards of other involved materials. General fire hazards No unusual fire or explosion hazards noted. 6. Accidental release measures Personal precautions, Keep unnecessary personnel away. Keep people away from and upwind of spill/leak.Wear protective equipment and appropriate protective equipment and clothing during clean-up.Do not touch damaged containers emergency procedures or spilled material unless wearing appropriate protective clothing. Ensure adequate ventilation. Local authorities should be advised if significant spillages cannot be contained. For personal protection, see section 8 of the SDS. Methods and materials for Large Spills: Stop the flow of material, if this is without risk. Dike the spilled material,where this is containment and cleaning up possible. Cover with plastic sheet to prevent spreading.Absorb in vermiculite, dry sand or earth and place into containers. Following product recovery,flush area with water. Small Spills:Wipe up with absorbent material(e.g. cloth, fleece). Clean surface thoroughly to remove residual contamination. Never return spills to original containers for re-use. For waste disposal, see section 13 of the SDS. Environmental precautions Avoid discharge into drains,water courses or onto the ground. 7. Handling and storage Precautions for safe handling Provide adequate ventilation. Do not get this material in contact with eyes. Avoid prolonged exposure. Wear appropriate personal protective equipment. Observe good industrial hygiene practices. Conditions for safe storage, Store in original tightly closed container. Store away from incompatible materials(see Section 10 including any incompatibilities of the SDS). 8. Exposure controls/personal protection Occupational exposure limits US.OSHA Table Z-1 Limits for Air Contaminants(29 CFR 1910.1000) Components Type Value ACETIC ACID(CAS PEL 25 mg/m3 64-19-7) 10 ppm US.ACGIH Threshold Limit Values Components Type Value ACETIC ACID(CAS STEL 15 ppm 64-19-7) TWA 10 ppm SOS US 2/7 US.NIOSH: Pocket Guide to Chemical Hazards Components Type Value ACETIC ACID(CAS STEL 37 mg/m3 64-19-7) 15 ppm TWA 25 mg/m3 10 ppm Biological limit values No biological exposure limits noted for the ingredient(s). Appropriate engineering Good general ventilation (typically 10 air changes per hour)should be used Ventilation rates controls should be matched to conditions. If applicable, use process enclosures,local exhaust ventilation, or other engineering controls to maintain airborne levels below recommended exposure limits. If exposure limits have not been established, maintain airborne levels to an acceptable level. Provide eyewash station. Individual protection measures,such as personal protective equipment Eye/face protection Wear safety glasses with side shields(or goggles)and a face shield. Skin protection Hand protection Wear appropriate chemical resistant gloves. Suitable gloves can be recommended by the glove supplier. Other Wear suitable protective clothing. Respiratory protection In case of insufficient ventilation,wear suitable respiratory equipment. Thermal hazards Wear appropriate thermal protective clothing,when necessary. General hygiene Always observe good personal hygiene measures,such as washing after handling the material considerations and before eating,drinking,and/or smoking. Routinely wash work clothing and protective equipment to remove contaminants. 9. Physical and chemical properties Appearance Physical state Liquid. Form Liquid. Color CLEAR Odor Vinegar Odor threshold Not available. pH Not available. Melting point/freezing point 61.88°F(16.6°C)estimated/999°F (537.22°C) Initial boiling point and boiling 213.59°F (100.89°C)estimated range Flash point 999.0°F (537.2 °C) Evaporation rate Not available. Flammability (solid,gas) Not applicable. Upper/lower flammability or explosive limits Flammability limit -lower Not available. (%) Flammability limit -upper Not available. (%) Explosive limit-lower(%) Not available. Explosive limit-upper(%) Not available. Vapor pressure 1.04 hPa estimated Vapor density Not available. Relative density Not available. Solubility(ies) Solubility(water) Not available. Partition coefficient Not available (n-octanol/water) Auto-ignition temperature 798.8`F (426"C)estimated SOS US 3/7 Decomposition temperature Not available. Viscosity Not available. Other information Explosive properties Not explosive. Flammability class Combustible IIIB estimated Oxidizing properties Not oxidizing. Percent volatile 100%estimated VOC (Weight%) 4.95%estimated 10. Stability and reactivity Reactivity The product is stable and non-reactive under normal conditions of use,storage and transport. Chemical stability Material is stable under normal conditions. Possibility of hazardous No dangerous reaction known under conditions of normal use. reactions Conditions to avoid Contact with incompatible materials. Incompatible materials Strong oxidizing agents. Hazardous decomposition No hazardous decomposition products are known. products 11. Toxicological information Information on likely routes of exposure Inhalation Prolonged inhalation may be harmful. Skin contact No adverse effects due to skin contact are expected. Eye contact Causes serious eye damage. Ingestion Expected to be a low ingestion hazard. Symptoms related to the Severe eye irritation. Symptoms may include stinging, tearing, redness, swelling,and blurred physical,chemical and vision. Permanent eye damage including blindness could result. toxicological characteristics Information on toxicological effects Acute toxicity Components Species Test Results ACETIC ACID(CAS 64-19-7) Acute Dermal LD50 Rabbit 1060 mg/kg Inhalation LC50 Guinea pig 5000 ppm, 1 Hours Mouse 5620 ppm, 1 Hours Rat 11.4 mg/I, 4 Hours Oral LD50 Mouse 4960 mg/kg Rabbit 1200 mg/kg Rat 3.31 g/kg Estimates for product may be based on additional component data not shown. Skin corrosion/irritation Prolonged skin contact may cause temporary irritation. Serious eye damage/eye Causes serious eye damage. irritation Respiratory or skin sensitization Respiratory sensitization Not a respiratory sensitizer. Skin sensitization This product is not expected to cause skin sensitization. Germ cell mutagenicity No data available to indicate product or any components present at greater than 0.1%are mutagenic or genotoxic. SOS US 4/7 Carcinogenicity This product is not considered to be a carcinogen by IARC, ACGIH, NTP,or OSHA. OSHA Specifically Regulated Substances(29 CFR 1910.1001-1050) Not listed. Reproductive toxicity This product is not expected to cause reproductive or developmental effects. Specific target organ toxicity- Not classified. single exposure Specific target organ toxicity- Not classified. repeated exposure Aspiration hazard Not an aspiration hazard. Chronic effects Prolonged inhalation may be harmful. 12. Ecological information Ecotoxicity The product is not classified as environmentally hazardous. However,this does not exclude the possibility that large or frequent spills can have a harmful or damaging effect on the environment. Components Species Test Results ACETIC ACID(CAS 64-19-7) Aquatic Crustacea EC50 Water flea(Daphnia magna) 65 mg/I,48 hours Fish LC50 Bluegill(Lepomis macrochirus) 75 mg/I, 96 hours * Estimates for product may be based on additional component data not shown. Persistence and degradability No data is available on the degradability of this product. Bioaccumulative potential Partition coefficient n-octanol /water(log Kow) ACETIC ACID -0.17 Mobility in soil No data available. Other adverse effects No other adverse environmental effects(e.g.ozone depletion, photochemical ozone creation potential, endocrine disruption,global warming potential)are expected from this component. 13. Disposal considerations Disposal instructions Collect and reclaim or dispose in sealed containers at licensed waste disposal site.Dispose of contents/container in accordance with local/regional/national/international regulations. Local disposal regulations Dispose in accordance with all applicable regulations. Hazardous waste code The waste code should be assigned in discussion between the user, the producer and the waste disposal company. Waste from residues/unused Dispose of in accordance with local regulations. Empty containers or liners may retain some products product residues. This material and its container must be disposed of in a safe manner(see: Disposal instructions). Contaminated packaging Since emptied containers may retain product residue, follow label warnings even after container is emptied. Empty containers should be taken to an approved waste handling site for recycling or disposal. 14. Transport information DOT Not regulated as dangerous goods. DOT information on packaging may be different from that listed. 15. Regulatory information US federal regulations This product is a"Hazardous Chemical"as defined by the OSHA Hazard Communication Standard,29 CFR 1910.1200. TSCA Section 12(b) Export Notification(40 CFR 707,Subpt.D) Not regulated. CERCLA Hazardous Substance List(40 CFR 302.4) ACETIC ACID (CAS 64-19-7) Listed. SARA 304 Emergency release notification Not regulated. SOS US 5/7 OSHA Specifically Regulated Substances (29 CFR 1910.1001-1050) Not listed. Superfund Amendments and Reauthorization Act of 1986 (SARA) Hazard categories Immediate Hazard-Yes Delayed Hazard-No Fire Hazard-No Pressure Hazard - No Reactivity Hazard - No SARA 302 Extremely hazardous substance Not listed. SARA 311/312 Hazardous No chemical SARA 313 (TRI reporting) Not regulated. Other federal regulations Clean Air Act(CAA)Section 112 Hazardous Air Pollutants (HAPs)List Not regulated. Clean Air Act (CAA)Section 112(r)Accidental Release Prevention (40 CFR 68.130) Not regulated. Safe Drinking Water Act Not regulated. (SDWA) US state regulations US.California Controlled Substances.CA Department of Justice(California Health and Safety Code Section 11100) Not listed. US. Massachusetts RTK-Substance List ACETIC ACID(CAS 64-19-7) US.New Jersey Worker and Community Right-to-Know Act ACETIC ACID(CAS 64-19-7) US.Pennsylvania Worker and Community Right-to-Know Law ACETIC ACID(CAS 64-19-7) US. Rhode Island RTK ACETIC ACID(CAS 64-19-7) US.California Proposition 65 California Safe Drinking Water and Toxic Enforcement Act of 1986 (Proposition 65): This material is not known to contain any chemicals currently listed as carcinogens or reproductive toxins. International Inventories Country(s)or region Inventory name On inventory(yes/no)* Australia Australian Inventory of Chemical Substances(AICS) Yes Canada Domestic Substances List(DSL) Yes Canada Non-Domestic Substances List(NDSL) No China Inventory of Existing Chemical Substances in China (IECSC) Yes Europe European Inventory of Existing Commercial Chemical Yes Substances (EINECS) Europe European List of Notified Chemical Substances(ELINCS) No Japan Inventory of Existing and New Chemical Substances(ENCS) Yes Korea Existing Chemicals List (ECL) Yes New Zealand New Zealand Inventory Yes Philippines Philippine Inventory of Chemicals and Chemical Substances Yes (PICCS) United States& Puerto Rico Toxic Substances Control Act(TSCA) Inventory Yes 'A"Yes'indicates that all components of this product comply with the inventory requirements administered by the governing country(s) A"No"indicates that one or more components of the product are not listed or exempt from listing on the inventory administered by the governing country(s). 16. Other information, including date of preparation or last revision Issue date 04-10-2015 SDS US 6/7 Revision date 05-10-2015 Version# 02 HMIS®ratings Health:3 Flammability:0 Physical hazard:0 NFPA ratings Health: 3 Flammability:0 Instability: 0 Disclaimer Amerochem cannot anticipate all conditions under which this information and its product, or the products of other manufacturers in combination with its product, may be used. It is the user's responsibility to ensure safe conditions for handling,storage and disposal of the product, and to assume liability for loss, injury, damage or expense due to improper use. The information in the sheet was written based on the best knowledge and experience currently available. Revision Information Hazard(s)identification: Prevention Physical and chemical properties: Color Physical and chemical properties: Oxidizing properties Physical and chemical properties: Odor Physical and chemical properties: Explosive properties Regulatory information: US federal regulations SOS US 7/7 APPENDIX D 22- ot3Z5 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing Solutions,Inc. Fax: (828) 350-9368 January 14, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16597 Test Start Date: 01-06-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Test Procedure, Method Number Result Code PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test v EPA-821-R-02-012, Method 2007.0 /� All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1)for the month in which it was performed, using the parameter code TGE3E. Additionally,the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATB(a ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, drn 41— Ji Sumner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 CITC Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing Solutions Inc Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: January 14, 2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP LaboratoryPerformin Test: Environmental Testing Solutions, Inc.,Certific ate#037 Comments Signature of Operator in Responsible Charge(ORC): ORC Phone/E-mail: Project#: 16597 Signature of Laboratory Supervisor: ,..t __.-- Sample#: 220106.11 e-Mail to: AT orms.ATBPncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 01-04-22 Organism Tested Collection Time: 0700 Test Start Date: 01-06-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration Control 7.79 7.66 pH (S.U.) X 23-h Treatment 7.64 7.90 7 X o n3 CO c Alkalinity(mg CaCO3/L) 100 Salinity(Initial/Adjusted)(ppt) 24.8 4.7/24.9 Control 7.9 7.7 D.O.(mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 8.0 7.6 Sample Temp.at Receipt(°C) 0.8 Mortality Replicate Mean Mortality Treatment 1 (Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2 (Exposure) A B C D Concentration Tested 90% 30% 20% 40% 30% 30.0% Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1 of 1 Acute Pass/Fail Whole Effluent Toxicity Test, Species: Americamysis bahia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES# NC0083321 Facility Hubert WTP Outfall 001 Project# I Co Sell County Onslow Test Concentration(Acute Limit) 90% Dilution mL mL Total volume Sample was not aerated or treated unless otherwise noted on this form.The sample was warmed to preparation: Sample Dilution water mL 25.0±1.0°C Ina warm water bath.Artificial sea salt was added to the sample to raise the salinity to 25.0±1.0 ppt.The sample was then diluted to the test concentration with salt synthetic water. 990 110 1100 Feeding Test Initiation or Termination Location Randomizing Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst incubator/Shelf Template 0 ' CIS30 t nw.,an 014,...01.•-0.... hgoh 1"Lo0 N 1 E ` P- 0' -1-2A 10(. I ( Ot-CS•1,1-- Zrd Ot.61.1'L 11.SSJA d termina Con 'Test organisms were fed in holding 2 to S hours prior to test initiation Test organisms were not fed during the test Chemical Analyses: •Analyst identified for each day,performed pH and dissolved oxygen measurements only.Temperature Concentration VC salinity performed at the time of test initiation or termination by the analyst performing the toxicity Initial Final test Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench Analyst (/ - k' sheets and transcribed to this bench sheet. pH(S.U.) (1iq /� �. - u(0 Chemical analyses: Control Dissolved oxygen(mg/L) /7 1 t W Parameter Reporting limit Method number Meter Serial number Salt SW 'Salinity(ppt) -LA• & 25'�I pH 0.1 S.U. SM 4500-H.8.2011 Accumet AR20 93312452 `Alkalinity(mg/L CaCO3) Dissolved/D� oxygen 1.0 mg/L SM 4500-0 G-2016 V51 Model 52CE 180104324 *Temperature(°C) �•-L m Conductivity 14.9 µmhos/c SM 2510 8-2011 Accumet AR20 93312452 t;.0 pH(S.U.) /4( I/ geto Salinity 1.0 ppt SM 2520 8-2011 Y51 PRO30 180104324 Dissolved oxygen(mg/L) ® Q �r/K^ Alkalinity 5.0 mg CaCO,/L SM 2320 8-2011 Accumet AR20 93312452 Test Concentration 'Salinity(ppt) `� _ Total residual y• `SsZ chlorine 0.1 mg/L ORION 97-70-1977 Accumet A8250 92349123 'Temperature(°C) —IS•, 'LS•s,( o4 Temperature 0.1°C SM 25508-2010 Digital Thermometer ': O bc c 100% pH(S.U.)100% 1. 1 Test Organism Information: in(salinity Dissolved oxygen(mg/L) Adjusted) 9. --- Organism Source: Aquatic Indicators,Inc. *salinity(ppt) - y.9 Batch(Al Batch Ab(: 01-03-22 pH(5.U.) '4r'1.t` Age(1 to 5 days old(: • l .�\1 S 100% Dissolved oxygen(mg/L) e � Date organisms were born: *Salinity(pot) 01-02-22 1200 to 01-03-22 1130 9.7 Conductivity(µmhos/cm( v e/9 0 Average transfer volume: <0.25 mL 'Total residual chlorine(mg/L) <6.10 Transfer bowl information: 7.41 0 pH(S.U.)= Temp.(°C)= ZS• Survival Data (number of living organisms): Control Test Concentration Statistics: Hours Method Replicate Replicate 1SJA� NSP A B C D E F G H t-stat or Rank M 3C 0 10 10 10 10 10 10 10 10 Initiation 1-tailed Critical 24 I 3 ( 0 I 0 (0 134 81A 644 11.4 PASS or FAIL A(k-..- Termination Mean survival: (001- Mean survival: 10 7- Comment codes: d=dead,u=unhealthy,s=stressed 50P AT41-Revision 5-Exhibit AT41.2 35 I Depot Street O Li Asheville.NC 28801 A AJ Phone: (828)350-9364 Fax: (828)350-9368 Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility: Environmental Chemists,Inc. NPDES#: NC0083321 Pipe a 001 County Onslow Hubert WTP Purchase order: Species: Americantysis(Mysidopsis)ba/tia Effluent dilution: 90% Test type: 24-hour Pass/Fail Acute Parameter code: TAA3E Sample information: (to be completed by sample collector) Composite sample: Sample location' 4-Mae n4 Start date: I--y -21. Time: O f O O Volume collected for testing y b End date: /- ( e2 a. Time: G°)o O Number of containers filled for testing: Number of samples per hour. ( Method of transport to laboratory: Enr,roch Gat Chilled during collection? yG5 Comments: If chilled,specify temperature: 3,"1°c. Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must be<6.0°C upon receipt at the laboratory. Sample custody: (to be completed by sample collector and facility personnel) BY SIGNING BELOW,I CERTIFY THAT THE PERMIT AND TEST REQUIREMENTS IDENTIFIED ON THIS FORM ARE ACCURATE Sample collected by: (Galen H l., hot AL&it-/ 07 O Print S,eaaec I)air:aM yin, 1I (^ `� .. Relinquished by: Received by: I!s Vrt o+t aK wea r+' Z1,,,(KtuJ,."--- 0 I9.5 Si 41.1 /�(r'Jki 0 S Y PnN 5quu,we Da,.un,.tin. Print }, i.u. 9.and tune ''Reelinquished hy: r Received by: �,.a o."LYi � als Ik_i.i �yw tx40 Print tiiluutw. Date and lime Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received at ETS by: ,n, cy ,1 1, q s, c,li U ab:and Custody seals intact?: LJ LJ Sample temperature upon receipt at ETS(°C): Cr* - Samples received in good condition?: Total residual chlorine upon receipt at ETS: EJ tEl (DPD Presence Absense Indicator,MDL 0 10 mg/L) Tracking number: I 01�" Project number: Sample number: Comments: - Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions,Inc. Source: Aquatic Indicators, Inc. IIIIIIIIIIIIIIIIIIII 0.54 - Control Limits (± 2 Standard Deviations) 0.52 - - • • • • • • 0.50 - • • • • • • • • • • • V 0.48 - • • • - Y J - j 0.46 - - O I I 1 I 1 I I I I I I I 1 I I I I I I I 0.65 L _ 0 0.60 - Warning Limits 00 0.55 - - 0.50 - • "• • • • • • • • •• •• • • • • - • • • • 0.45 - - 0.40 - - 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 06 Oti 01 01 06 09.15 10.06 PlA''1�A$ 105 01.01 03 Oti 0A.O6 05 04 06' 01' 0a 03 09.1a 1.05 1 Oti 01 .OA L1 Test date • 48-hour LCS0=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to 50%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LC50 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LCso±SA.10 converted to anti-logarithmic values, SA 10=10th percentile of CVs reported nationally by USEPA) ww..a a...w we.« 22-0.352q PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental resting Solutions,Inc. Fax: (828) 350-9368 February 19, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16715 Test Start Date: 02-09-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Result Test Procedure, Method Number Code PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test " EPA-821-R-02-012, Method 2007.0 J� All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1) for the month in which it was performed, using the parameter code TGE3E. Additionally, the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATBncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, t�1 Jim umner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing solutions I°< Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: February 19, 2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions, Inc.,Certificate#037 Comments Signature of Operator in Responsible Charge(ORC): . ORC Phone/E-mail: Project#: 16715 Signature of Laboratory Supervisor: �r/1(,7rC�t►��,Q�,�_ Sample#: 220209.13 e-Mail to: ATFlo/rms.ATB@ncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 02-07-22 Organism Tested Collection Time: 0720 Test Start Date: 02-09-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration Control 8.00 OE c c pH(S.U.) X 23.5-h s0 Treatment 7.94 0 x o r° t= Alkalinity(mg CaCO3/L) 100 v3 LL' Salinity(Initial/Adjusted)(ppt) 24.9 5.4/25.1 Control ®® D.O.(mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 8.0 ED Sample Temp.at Receipt(°C) 1.1 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration Tested 90% 60% 80% 60% 80% 70.0% Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS . Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1 of 1 Acute Pass/Fail Whole Effluent Toxicity Test,Species: Americamysis bahia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES# NC0083321 Facility Hubert WTP Outfall 001 Project# ►lo'\k S County Onslow Test Concentration(Acute Limit) 90% Dilution mL mL Total volume Sample was not aerated or treated unless otherwise noted on this form.The sample was warmed to preparation: Sample Dilution water mL 25.0 S 1.0°C in a warm water bath.Artificial sea salt was added to the sample to raise the salinity to 25.0 2 1.0 ppt.The sample was then diluted to the test concentration with salt synthetic water 990 110 1100 Hours Date Feeding Test Initiation or Termination Location Randomizing Sample Number Salt SW Batch Time Analyst Time Analyst Incubator/Shelf Template 0 ' 05.10 4 ,,,,,,°° 07 °7 t7 ICOQ 17fp A-( G 0 0/..le 1101oat. (� Di-07•I1B 24 _ rrrr,naii r CA-At Lt 121 0 A•( •Test organisms were fed In holding 2 to 5 hours prior to test Initiation.Test organisms were not fed during the test Chemical Analyses: -Analyst identified for each day,performed pH and dissolved oxygen measurements only. Temperature and salinity performed at the time of test initiation or termination by the analyst performing the toxicity Initial Final test.Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench Analyst �{ LIC Concentration N`\,( sheets and transcribed to this bench sheet. pH(S.U.) a•po '•S2 Chemical analyses: Dissolved oxygen(mg/L) Parameter Reporting limit Method number Meter Serial number Control ,., ',� Salt SW *Salinity(ppt) pH 0.1 S.U. 5M 4500-H.8-2011 Accumet AR20 93312452 •Alkalinity(mg/L CaCO3) 100 Dissolved oxygen 1.0 mg/L SM 4500-0 G-2015 Y51 Model 52CE 180104324 'Tem erature 1°C) �lar'q-. p (° ) Mt) 'IS- Conductivity 14.9 µmhos/cm SM 2510 8.2011 Accumet AR20 93312452 pH(S.U.) , S \ /Y 1,I Salinity 1.0 pot SM 25208-2011 Y51 PR030 18D104324 Dissolved oxygen(mg/L) a•0 r4xVw Alkalinity 5.0mgCaCO,/L SM 2320 8-2011 Accumet AR20 93312452 Test Concentration •Salinity(ppt) 9 t/ 'ISO) Total residual 0.1 mg/L ORION 97-70-1977 Accumet A8250 92349123 l 7 �Jrs 7 chlorine 'Temperature 1°C) ,,JJ Temperaturej y Z-r.S 15.� P 0.1°C SM 25508-2030 Digital Thermometer l 066 01' 100% pH(S.U) 1•ate Test Organism Information: (Salinity Dissolved oxygen(mg/L) 1 % Organism Source: Aquatic Indicators,Inc. Adjusted) 'Salinity(ppt) 2r•I Batch(Al Batch Ab): 02-07-22 pH(S.U.) 1• $L Age(1 to 5 days old): .1_ DAA.S Dissolved oxygen(mg/L) Date organisms were born: 100% 1• *Salinity(ppt) 02-06-22 1200 to 02-07-22 1130 S•y Conductivity(umhos/cm) Average transfer volume: <0.25 mL ADC) 'Total residual chlorine(mg/L) GQ Jo Transfer bowl information: pH(5.u.)= -.Qt. Temp.(°C)= AS.0 Survival Data (number of living organisms): Control Test Concentration Statistics: Hours Replicate Replicate Method Vrjv..//We( A B C D E F G H t stat or Rank Nr 0 10 10 10 10 10 10 10 10 i Initiation 1-tailed Critical N/R 24 ) o p 0 1 0 y 641 0y a2 QJ PASS or FAIL F—,./ Termination Mean survival: 1001' Mean survival: 30 y, Comment codes: d o dead,u=unhealthy,s=stressed SOP AT41-Revision 5-Exhibit AT41.2 /ue-s A 0 $ L /�` 351 Depot Street v Asheville,NC 28801 Phone: (828)350-9364 Fax: (828)350-9368 • Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility: Environmental Chemists,Inc. NPDES#: NC0083321 Pipe#: 001 County: Onslow Hubert WTP Purchase order: Species: Americamysis(Mysidopsis)ba/lia Effluent dilution: 90% Test type: 24-hour Pass/Fail Acute Parameter code: TAA3E Sample information: (to be completed by sample collector) ' Composite sample: Sample location: L.11,.l rP CON ' .a 4 Start date: 07`7-2 R Time: C'yS f Volume collected for testing N L. End date: cl- V-.2 3- Time: 0 7 ZO Number of containers filled for testing: I Number of samples per hour: t 1 Method of transport to laboratory: t n vs?sac h.e_,,w Chilled during collection? y,e fr Comments: If chilled,specify temperature: 3. 3 Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must be<6.0°C upon receipt at the laboratory. Sample custody: (to be completed by sample collector and facility personnel) BY SIGNING BELOW,I CERTIFY THAT THE PERMIT AND TEST REQUIREMENTS IDENTIFIED ON THIS FORM ARE ACCURATE Sample collected by: dt\0 ri titAiiieAviar jiaikie fall - Pnnt Signature Dew.11tins Relinquished by: Received by: i9" kY b ,LIs•p-.G5)o13Q, -Slotti Stgt Pitb-A2:52 Pnnt tip,atu c Date end umc Rats atue 0.tc.nd time. e� "" Relinquished by: Received by: TF1 txc V - 2 $ 22 io23 - '" '~ Not L Dee and nms Pnm Signature Deis and ttmc Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received at ETS by: ECPI.(‘ OZ�o 2" 04, Q 1-0iUol: Pool tigmius Date and ume Pnnt Sip,aiue Dam,and ttmc Custody seals intact?: n = = Sample temperature upon receipt at ETS(°C): Ye No Not used 141 'L Samples received in good condition?: [ n Ye No Total residual chlorine upon receipt at ETS: EJ (DPD Presence Absense Indicator,MDL 0 10 mg/L) P1va11 At'''' Tracking number: 14 ��U�Project number:1 l,�tjSample number: UM.7 1 f Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions,Inc. Source: Aquatic Indicators, Inc. I I I I I I I I 1 I I I I I I 1 I 1 0.54 - Control Limits (± 2 Standard Deviations) 0.52 - • • • • • • • 0.50 - • • • • - • • • • 0.48 - • • • J - - " 0.46 - - I I I I I I I I I I I I I I I I I I I J 0.65 I I I I I I I I I I I 1 I I I I I I I I O 0.60 - Warning Limits t 00 _ 0.55 - - • • • • • 0.45 - - 0.40 - - Oa,11�9,15.,0.0 11.03.1ti.0a��.OS�ti.Oti o3.Oti�Q.06.oSOa.06.0$0�,13�a.03�9.1°.L�AS 1.Oti ti 01"OlAQ.OL.Oa-OL,16 Test date • 48-hour LC50=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to 50%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LC50 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LC50±SA 10 converted to anti-logarithmic values, SA 10= 10`h percentile of CVs reported nationally by USEPA) imsem R T 2 2 - �s 3° PO Box 7565 Asheville, NC 28802 Phone: (828)350-9364 Environmental Testing Solutions,Inc Fax: (828)350-9368 March 17, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16805 Test Start Date: 03-09-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Result Test Procedure, Method Number Code PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test v EPA-821-R-02-012,Method 2007.0 • /� All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1)for the month in which it was performed, using the parameter code TGE3E. Additionally,the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATBCr.�ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, O Ji Sumner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: March 17, 2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions, Inc., Certificate#037 Comments Signature of Operator in Responsible Charge(ORC): ORC Phone/E-mail: Project#: 16805 Signature of Laboratory Supervisor: ` � Sample If: 220309.17 e-Mail to: AT orms.ATB@ncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 03-07-22 Organism Tested Collection Time: 0738 Test Start Date: 03-09-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration Control 7.86 8.06 X 24-h o pH(S.U.) Treatment 7.86 7.99 ° Alkalinity(mg CaCO3/L) 100 n c" Salinity(Initial/Adjusted)(ppt) 25.2 5.5/25.0 Control 7.8 7.7 D.O. (mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 7.6 7.8 Sample Temp.at Receipt(°C) 2.0 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration Tested 90% 40% 60% 50% 80% 57.5% Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1 of 1 Acute Pass/Fail Whole Effluent Toxicity Test, Species: Americamysis bahia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPOES# NC0083321 Facility Hubert WTP Outfall 001 Project# 1 tag OS County Onslow Test Concentration(Acute Limit) 90% Dilution mL nit Total volume Sample was not aerated or treated unless otherwise noted on this form,The sample was warmed to preparation: Sample Dilution water mL 25.0 2 1.0°C in a warm water bath.Artificial sea salt was added to the sample to raise the salinity to 25.0!1.0 ppt. The sample was then diluted to the test concentration with salt synthetic water. 990 110 1100 Feeding Test Initiation or Termination Location Randomizing Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst incubator/shelf Template InInIt- �n°n a .o't•2L ' os o900 1:-k A'S \� La)tir� 12t>30gx1"1 (Jb 6'�2t%k 24 t„..„bo, n•10.11- Vest organisms were fed in holding 2 to 5 hours prior to test Initiation.Test organisms were not led during the test Chemical Analyses: •Analyst identified for each day,performed pH and dissolved oxygen measurements only.Temperature and salinity performed at the time of test initiation or termination by the analyst performing the toxicity V v VC Initial Final test.Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench Analyst �t Concentration ' l n / it/ sheets and transcribed to this bench sheet. pH(S.U.) 7-PJl4 ,0(0 Chemical analyses: Control Dissolved oxygen(mg/L) ,8 ,1e 1- Parameter Reporting limit Method number Meter Serial number Sail SW `Salinity(pet) 1,-5•2 2.7)8 pH 0,1 S.U. 5M 4500-H♦8.2011 Accumet AR20 93312452 `Alkalinity(mg/L CaCO3) 1 00 Dissolved oxygen 1.0 mg/L SM 4500-0 G-2016 YSI Model 52CE 180104324 •Temperature(°C) �• - 'LS•1— Conductivity 14.9 µmhos/cm 5M 2510 B-2011 Accumet AR20 93312452 pH(S.U.) —7ya v4 60 Salinity 1.0 ppt SM 2520 B-2011 Y51 PR030 18D104324 �' Dissolved oxygen(mg/L) , 'd Alkalinity 5.0 mg CaCO5/L SM 2320 B-2011 Accumet AR20 93312452 Test (/ Concentration *Salinity(ppt) 2.5-0 2?xL( Total residual chlorine 0.1 mg/L ORION 97-70-1977 Accumet A32S0 92349123 °Temperature(°C) AS A As- L- Temperature 0.1°C SM 2550B-2010 Digital Thermometer ‘3061011665 pH(S.U.) No% 7 p Test Organism Information: (salinity Dissolved oxygen(mg/L) - •e Organism Source: Aquatic Indicators,Inc. Adjusted) 'Salinity(ppt) 2,CD Batch(Al Batch Ab): 03-07-22 pH(S.U.) 7 Y5 Age(1 to 5 days old): —L 3 ` iKAS Dissolved oxygen(mg/L) �J! Date organisms were born: 100% *Salinity(ppt) 03-06-22 1200 to 03-07-22 1130 Conductivity((,mhos/cm) q9 OilV Average transfer volume: <0.25 mL • °Total residual chlorine(mg/L) . 1OTransferbowlinformation: PH(SM.). $.1� Temp.(°C)= Z.�•�L t Survival Data (number of living organisms): Control Test Concentration sraristics: Hours Replicate Replicate Method VIS4At_, iOSP A B C D E F G H t-stat or Rank tJC 0 10 10 10 10 10 10 10 10 Initianon 1 tailed Critical IJC 24 / yd 6J r 1 L d gd 10 /o /0 /O b ti S ? PASS or FAIL Fis Termination Mean survival: /o0•l- Mean survival: `{•L %Z_ Comment codes: d=dead,u=unhealthy,s=stressed SOP AT41-Revision 5-Exhibit AT41.2 /164 35I Depot Street yM Asheville,NC 28801 / Phone: (828)350-9364 Fax: (828)350-9368 Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility: Environmental Chemists,Inc. NPDES s<: NC0083321 Pipe sl: 001 County: Onslow Hubert WTP Purchase order: Species: Americamysis(Mysidopsis)bairia Effluent dilution: 90% Test type: 24-hour Pass/Fail Acute Parameter code: TAA3E Sample information: (to be completed by sample collector) Composite sample: Sample location reg10e10Yf Start date: _3- 7. 1 - Time 0 9 33 Volume collected for testing 4 L End date: 3. 8. 2.2 Time 0 7 3 Y Number of containers filled for testing: Number of samples per hour: I Method of transport to laboratory: Ert v,Srpc he Chilled during collection? ye J' Comments If chilled,specify temperature: 3,1 Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must be<6.0°C upon receipt at the laboratory. Sample custody: tto be completed by sample collector and facility personnel) BY SIGNING BELOW,I CERTIFY THAT THE PERMIT AND TEST REQUIREMENTS IDENTIFIED ON THIS FORM ARE ACCURATE Sample collected by: s•k' z� Ga1e 1'‘4.7r10er Auk Idiq,i444,1 ovtia Pnnt Stamm. Relinquished by: Received by: k• 32 S/!/L t.a•A h t,3e0e4- 1��6^p,1,�N 4)w- 0939 I'nnt Stpnature Da,asd um. ,r.i ltpruture Date and tar Relinquished by: 'Received by: ,a Inn, *natter Due and um, .i 1tp,uture Date and mac Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received at ETS by: C3. 2t 03.09.22 L CL.e.n ell nrt/ v O j(r- ✓t- l'nnt Print S oats t6 Stprutun [btc arW ItrtrSquatter and nuns Custody seals intact?: 1=1 Sample temperature upon receipt at ETS(°C): MI Yea No Nnt used Samples received in good condition?: Yea No Total residual chlorine upon receipt at ETS: Q (DPD Presence Absense Indicator,MDL=0 10 mg/L) lt""e"' Al'f1M Tracking number: 1**1 ������ Project number:'/ Sample number: Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions Inc. Source: Aquatic Indicators, Inc. 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 0.54 - Control Limits (± 2 Standard Deviations) 0.52 - - • • • • • • • 0.50 - • • • - • • • • • • • - V 0.48 - • • • - Y J - - ba 0.46 - - I 1 I l I I I 1 I I 1 I I I l I I I I 1 Si 0.65 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 G 0.60 - Warning Limits s 00 0.55 - - • 0.50 - • • •• • • • • • • • • • • • • • • • • 0.45 - - 0.40 - - 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 ,�S.'L0 06*0 0-N- 0S 10 OS 11 01 11 0.1 06�1 Op Ll��11 1311 03.11 1a�1 os.1 v oti�101�1 os" oa 1ti S Lti oS Lti 09 IP- A). L1 01 01; 0g• op• 0S- 06' 01 04) 09' IP' 11' 11' OY 01.' p1' 03' Test date • 48-hour LC50=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to 50%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LCS0 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LC50±SA 30 converted to anti-logarithmic values, SA 10=10th percentile of CVs reported nationally by USEPA) mutt tne rutonoe by w.w.Mw T ,ram a. PO Box 7565 Asheville, NC 28802 Phone: (828)350-9364 Environmental Testing Solutions.Inc. Fax: (828)350-9368 March 28,2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16821 Test Start Date: 03-22-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter *Result Code Test Procedure, Method Number PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test V EPA-821-R-02-012, Method 2007.0 /� *Test was invalidated. Associated reference test was above control limits,suggesting that the organisms lacked sensitivity. All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1)for the month in which it was performed, using the parameter code TGE3E. Additionally,the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATB@ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, umner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 • EnNronmonUl Teeing SOluuons,Inc Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: March 28,2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions,Inc.,Certificate#037 Comments Invalid test due to Signature of Operator in Responsible Charge(ORC): outlier reference test. ORC Phone/E-mail: Project#: 16821 Signature of Laboratory Supervisor: V yr it-e - Sample#: 220322.01 e-Mail to: A Forms.ATB(a)ncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 03-20-21 Organism Tested Collection Time: 0859 Test Start Date: 03-22-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration p Control 8.12 8.01 . X 26.25-h o H(S.U.) Treatment 7.97 7.92 X O F- ,_ -0 (D c Alkalinity(mg CaCO3/L) 120 in La Salinity(Initial/Adjusted)(ppt) 25.3 5.3/25.0 Control 7.7 7.4 D.O.(mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 8.0 7.5 Sample Temp.at Receipt(°C) 2.6 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration 90% 36.4% 20% 40% 30% 31.6% Tested Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS . Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 I .r Page l of 1 Acute Pass/Fail Whole Effluent Toxicity Test,Species: Americamysis bahia I EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES t# NC0083321 1 Facility Hubert WTP Outfall 001 Project II LID E2 J County Onslow I Test Concentration(Acute Limit) 90% Dilution mL mL Total volume Sample was not aerated or treated unless otherwise noted on this form.The sample was warmed to preparation: Sample Dilution water mL 25.0±1.0°C in a warm water bath.Artificial sea salt was added to the sample to raise the salinity to I 25.0 t 1.0 ppt.The sample was then diluted to the test concentration with salt synthetic water. 990 110 1100 I i Feeding Test Initiation or Termination Location Randomizing Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst Incubator/Shelf Template in,P�r,°° t53--1.1•11_ 11OS (aS K 11 I A-f `L C. sL')e_. -1:2_0 --•L.O` 03-\VII_ 24 tr,m °^ 03•vs•2'L IYST 4•( I 'Test organisms were fed in holding 2 to S hours prior to test initiation.Test organisms were not fed during the test. Chemical Analyses: •Analyst identified for each day,performed pH and dissolved oxygen measurements only.Temperature and salinity performed at the time of test initiation or termination by the analyst performing the toxicity test. Initial Final Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench sheets I Concentration �y,�/ and transcribed to this bench sheet. Analyst V v' fa•S pH(S.u.) �d g.0� Chemical analyses: Dissolved oxygen(mg/L) 7,7 -1•-k Parameter Reporting limit Method number Meter Serial number I Control Salt SW W`udr fi *Salinity(pp[) �'� n•,_C L 7 2?N. pH 0.15.U. SM 4500-He 8.2011 Accumet AR20 93312452 *Alkalinity(mg/L CaCO5) t 2� '7 Dissolved oxygen 1.0 mg/L SM 4500-0 G-2016 YSI Model 52CE 180104324 I *Temperature('Cl —LA.b ZS•O Conductivity 14.9 µmhos/cm SM 2510 B-zou Accumet AR20 93312452 pH(S.U.) 91 7 9 7 Salinity 1.0 ppt SM 2520 B-2011 Y51 PRO30 180104324 Dissolved oxygen(mg/L) ( 0 S Alkalinity 5.0 mg CaCO5/L SM 2320 B-2011 Accumet AR20 93312452 Test Concentration *Salinity(ppt) —LS•1*-- 7 t•/ Total residual chlorine 0.1 mg/L ORION 97-70-1977 Accumet A8250 92349123 *Temperature(°C) �` `ZS-.Q Temperature 0.1°C SM 25500-2010 Digital Thermometer 13(Ib�a�6r1�y pH(S U.) -`�, 100% !-I Test Organism Information: (salinity Dissolved oxygen(mg/0 l'i3O Organism Source: Aquatic Indicators,Inc. Adjusted) I *Salinity(ppt) Batch(Al Batch Ab) 03-21-22 —LS•O pH(S.U.) �v-�j5 Age(1 to 5 days old): 1-^L Amy Dissolved oxygen(mg/L) c O I Date organisms were born: 100% `Salinity(ppt) ( 03-20-22 1200 to 03-21-22 1130 '�� G 1.G oS.ttzt� Conductivity(µmhos/cm( C1SO Average transfer volume: <0.25 mL "1-A,-to �_1b *Total residual chlorine(mg/L) < 0-to Transfer bowl information: pH(Std.), Temp.(°C1= 4� 8.zS �l!L Survival Data (number of living organisms): Control Test Concentration Statistics: Hours Method Ut N)Pl. I►*3SP Replicate Replicate 1 A B C D E F G H t-stat or Rank 1 0 /r O1 Pa N C, 10 10 10 10 .194 j 10 10 10 1-tailed Critical t✓ IInitiation ol•11-?5.q.. / C24 /Q r0 /Q (0 - ,j 8Zj t 73dPASS or FAIL 1-A%L Termination Mean survival: /p0/. Mean survival: 6g-y 7. 1 Comment codes: d=dead,u=unhealthy,s o stressed SOP AT41-Revision 5-Exhibit AT41.2 L L 351 Depot Street Asheville,NC 28801 Phone: (828)350-9364 Fax: (828)350-9368 - Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility: Environmental Chemists,Inc. NPDES if: NC0083321 Pipe if 001 County: Onslow Hubert WTP Purchase order: Species: Americamysis(Mysidopsis)bahia Effluent dilution: 90% Test type: 24-hour Pass/Fail Acute Parameter code: TAA3E Sample information: (to be completed by sample collector) Composite sample: Sample location: (-4 t!/ P E•1-F/ C.:r enT Start date ?j—2 0 —7 2 Time: 06 it Volume collected for testing: y L End date: 3-3 I _Z 7 Time: (j 5 g Number of containers filled for testing: f Number of samples per hour: I Method of transport to labors ry: Er)L,fo di e/n Chilled during collection? Y es Comments �r.��jrf If chilled,specify temperature: . , y "< Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must be<6.0"C upon receipt at the laboratory. Sample custody: (to be completed by sample collector and facility personnel) Sample collected by: I Ci Q CJQ CGtrrstop er 3-Z l-Zz. Prim Swann.: late and tune �+ Relinquished by: Received/� by: ) 'p•A/� 1 — / 09`►5 L.C.?'� se.* hrJil �'` ,( (S )a.'L '. kr,y=urh er-�Iedf/, 3`2 i-- �� ' _ / 5 Pnnt Sigmaturo Dale and Min Pont srrnmmo \ Date andiim Relinquished by: Received by: qc CAA (f�1\•1.t 6ttdti,k we her 3 .z r A 7 Ceoe4- CC:1 rr"re" 1412,.J 4 1^ l r A 2 Print Swan.: Dab:and time Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received at ETS by: fib'11•art., t1 .-1. . vl-cNed, Trim siEnatare Dam and Mne Prim Sigmmrs Date and time tty-1L 1l Custody seals intact?: '-/1( n -p�- J' 1 N Sample temperature upon receipt at ETS("C): Yc. No Not u.d Samples received in good condition?: v/ n Von No Total residual chlorine upon receipt at ETS: 74/ (DPD Presence/Absense Indicator,MDL=0.10 mg/L) Pm«m Ahem Tracking number: k jlo • 0\3 St L(r, gII-- Project number!`i 2't Sample number:Z203 Z2,()l Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions,Inc. Source: Aquatic Indicators, Inc. M M I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 0.58 - - • 0.56 - Control Limits (± 2 Standard Deviations) _ 0.54 - - 0.52 - - • • • • • • • 0.50 - • • • • — • • • • • 0.48 — • • • - V - Y 0.46 - - J -to 0.44 - - 1 i 1 1 1 1 V 0.65 1 I 1 1 1 1 1 I I 1 1 I 1 1 1 1 1 1 1 I L t 0.60 - Warning Limits ob ..• - 0.55 - .___/• - • • • • • • • _ 0.40 - - 061°051°061°0511 0.1.0111 00>0Q11 D811 1311 0 31.1Q 11 0511 A.:11 0�11 Da 11 0$ '1 1611 001—1L1L11- 1°. 11. ,11 01. 01- OS. ON. 05. 06' 01. OS- O9. 10- ,11 11. 01 01. 01- Olf O3 Test date • 48-hour LC50=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to S0%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LC50 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) .. Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LC50±SA 10 converted to anti-logarithmic values, SA 10=10th percentile of CVs reported nationally by USEPA) tnN aM dvwC by J.SI MMI 22-012O 4 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing Solutions.Inc. Fax: (828) 350-9368 April 15, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16884 Test Start Date: 04-06-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Result Code Test Procedure, Method Number PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test EPA-821-R-02-012,Method 2007.0 X All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1)for the month in which it was performed, using the parameter code TGE3E. Additionally,the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATB(a ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, Jimc *fr e Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 EnNmnmenul Testing Solution%Inc. Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: April 15, 2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions, Inc., Certificate#037 Comments Signature of Operator in Responsible Charge(ORC): ORC Phone/E-mail: Project a: 16884 Signature of LaboratorySupervisor: ( 1. t .�"IQ-- Sample 4: 220406.32 e-Mail to: ATForms.ATBPncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 04-04-22 Organism Tested Collection Time: 0830 I Test Start Date: 04-06-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration Control 8.00 8.02 . X 25-h o r pH(S.U.) _ Treatment 7.92 7.98 ,7 f0 C Alkalinity(mg CaCO3/L) 130 v '-'' Salinity(Initial/Adjusted)(ppt) 24.8 4.7/24.6 Control 7.6 7.6 D.O.(mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 8.0 7.8 Sample Temp.at Receipt(°C) 2.9 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration 90% 70% 60% 60% 60% 62.5% Tested Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1 of 1 Acute Pass/Fail Whole Effluent Toxicity Test,Species: Americamysis bahia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES# NC0083321 Facility Hubert WTP Outfall 001 Project# 11.E f 4 County Onslow Test Concentration(Acute Limit) 90% Dilution nil mL Total volume Sample was not aerated or treated unless otherwise noted on this form.The sample was warmed to preparation: Sample Dilution water mL 25.0 3 1.0°C In a warm water bath.Artificial sea salt was added to the sample to raise the salinity to 25.0 3 1.0 ppt.The sample was then diluted to the test concentration with salt synthetic water. 990 110 1100 Feeding Test Initiation or Termination Location Randomizing Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst incubator/Shelf Template 0 • ()Cf)Lr U o o•(.a�•In— two ,z�11 Al. 1-0 ‘ot\vTe "1.1o`10b. bL u3-3o•1.1.4 24 \t.i R ,7 ,ram+°.ri°° 0`�.lJl.1-L a\(` 'Test organisms were fed In holding 2 to 5 hours prior to test initiation.Test organisms were not fed during the test Chemical Analyses: 'Analyst dent fied for each day,performed pH and dissolved oxygen measurements only.Temperature and salinity performed at the time of test initiation or termination by the analyst performing the toxicity test. Initial Final Alkalinity and total residual chlorine performed by the analysts Identified on the test specific bench sheets Concentration Analyst q I' V1/ and transcribed to this bench sheet. X pH(S.U.) 7.0O an- Chemical analyses: Dissolved oxygen(mg/L) 1•b Reporting limit Method number Meter Serial number Control , Parameter Salt SW `Salinity(opt) 1`1 ' r 6_ Z T.S.0 m pH 0.1 S.U. SM 4500-H+B-2011 Accumet AR20 93312452 1 'Alkalinity(mg/L CaCO,) `-a,0 Dissolved oxygen 1.0 mg/L SM 4500-0 G-2016 YSI Model 52CE 180104324 'Temperature(°C) —1.A C\ 'AS,0 Conductivity 14.9pmhos/cm SM2510B-2011 AccumetAR20 93312452 pH(s.u.) y? Salinity 1.0 opt 5M 2520 0.2011 YSI PRO30 160104324 Dissolved oxygen(mg/L) 8. 0 .1--0 `0 Alkalinity 5.0 mg CaCO,/L SM 2320 5.2011 Accumet AR20 93312452 Test 7 Concentration 'Salinity(put) Total residual chlorine 0.1 m L ORION 97.70.1977 Accumet A0250 92349123 zy.l, t.�, S � 'Temperature(°r) ` 1S ` Temperature 0.1°C SM 2550B-2010 Digital Thermometer 1 A041,1 1,IS 100°4 pH(S.u.) 7a y/ Test Organism Information: (Salinity Dissolved oxygen(mg/L)Adjusted) 6(`•‘) Organism Source: Aquatic Indicators,Inc. 'Salinity(pot) Zit,(a Batch(Al Batch Ab): 04-04-22 pH(OAT) 7 )a 6 Age(i to 5 days old): 1—'J t.ty\t s Dissolved oxygen(mg/L) Date organisms were born: 100% &.L) 04-03-22 1200 to 'Salinity(ppt) 04-04-22 1130 Conductivity(µmhos/cm) a'4l 0 Average transfer volume: <0.25mL 'Total residual chlorine(mg/L) <0.10 Transfer bowl information: pH(S.U.)= g.Os Temp.(°C)u it(./ Survival Data (number of living organisms): Control Test Concentration Statistics: Hours Method sJ c p , itsie Replicate Replicate A B C D E F G H t-stat or Rank IJL 0 10 10 10 10 10 10 10 10 Initiation 1-tailed Critical 24 (0 /0 i 0 (Q 3 t_t�A �yd `�Li PASS or FAIL PA►L Termination Mean survival: 1001. Mean survival; ,n.S 1. Comment codes: d=dead,u=unhealthy,s=stressed SOP AT41-Revision 5-Exhibit AT41.2 • Cs • ��•- At C • 351 Depot Street Asheville,NC 28801 Phone: (828)350-9364 -) — ' - Far: (828)350-9368 Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility Environmental Chemists,Inc. NPDES# NC0083321 Pipe# 001 County Onslow Hubert WTP Purchase order Species Antericantysis(Mysidopsis)bahia Effluent dilution 90a/o Test type 24-hour Pass/Fail Acute Parameter code TAA3E Sample information: (to be completed by sample collector) L Composite sample: Sample location r'u be r f t,,TP E 6`,1N0 t Start date H- -w - Time 0 j- 2 C a,^ Volume collected for testing 1 L End date it_tj- 20 : Time a' .- 3 0 cL of Number of containers filled for testing I Number of samples per hour 'I Method of transport to laboratory En(i:ro ale/n Chilled during collection J e Comments If chilled,specify temperature 3,g °C Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must he<6.0"C upon receipt at the laboratory. Sample custody: Ito be completed by sample collector and facility personnel) Sample coikcted by: Chi 51114 Hu oM 5 -Z` tt"t s,—,-- Dr..tnJ vmc Relinquished by: Received by: 6-_yo,.. .v�h���$1 y i3� -Tom 13EA5Le`r 'y' 121 Relinquished by: Received by: -Ihtnl stpmlurt Doe and tune Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received Si EIS by: Eti—ern at,,,,,,, i, oy.0..Lt. tool stpMturt end"me 1'nn sigtulurt Doe eml nine Custody seals intact?: = -F, Sample temperature upon receipt at ETS("C): 21 v Ye N Nd urJ Samples received in good condition?: Ye Nn Total residual chlorine upon receipt at ETS: E (DPD PresenceiAbsense Indicator hmL-r:11'in.:Li Tracking number: t, „,a / 2 �ws�� Project number. Sample number: vY/ Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Tasting Solutions.Inc. Source: Aquatic Indicators, Inc. 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 0.58 - - 0.56 - Control Limits (± 2 Standard Deviations) 0.54 - • • - 0.52 - - • 0.50 - • • • • • • • • • •- • • • 0.48 - • • U - - Y 0.46 - - 0- 0.44 - - 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 J 0.65 I I I I I 1 I I I I I 1 1 I I I 1 I I L _ a 0.60 - Warning Limits s 00 a vt 0.55 - • • - • • 0.50 • • • • • • • • • • • • • • • 0.45 - - 0.40 - - I 1 I 1 I 1 I I I 1 1 1 1 1 1 1 1 1 1 I 0105�tiO3 03 Oti Op.06�S 0��6 0$�1.L'':IN IN�91a 0 os 1�Oti�ti 01��ow Oti os�ti 16 Q3.os�3..1; .0s.oet A os�4.01-� Test date • 48-hour LC50=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to 50%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LC50 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LCS0±SA iO converted to anti-logarithmic values, SA 10=10th percentile of CVs reported nationally by USEPA) inrdevaned nw.n. nnsannw V- 22 rc V�O PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing Solutions,Inc. Fax: (828) 350-9368 April 25, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16920 Test Start Date: 04-19-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Result Test Procedure, Method Number Code PASS FAIL Americamysis Pass/Fail Acute Toxicity Test TGE3E X EPA-821-R-02-012, Method 2007.0 • All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1) for the month in which it was performed, using the parameter code TGE3E. Additionally, the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATBna ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, Ji Sumner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Fax: (828) 350-9368 Effluent Toxicity Report Form -Acute Pass/Fail Date: April 25, 2022 Facility: Environmental Chemists, Inc. NPDES#: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions, Inc.,Certificate#037 Comments Signature of Operator in Responsible Charge(ORC): ORC Phone/E-mail: Project a: 16920 Signature of Laboratory Supervisor: c iy/4— Sample u: 220419.01 e-Mail to: ATForms.ATB@ncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 04-17-22 Organism Tested Collection Time: 0730 Test Start Date: 04-19-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration Control 8.26 11111 c c pH(S.U.) X 24.25-h s Treatment 8.07 7.94 _z x FO L Alkalinity(mg CaCO3/L) 130 w Salinity(Initial/Adjusted)(ppt) 24.7 5.9/25.0 Control ®® D.O.(mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 7.6 LEI Sample Temp.at Receipt(°C) 0.9 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration 90% 70% 70% 90% 60% 72.5% Te sted Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1 of 1 Acute Pass/Fail Whole Effluent Toxicity Test, Species: Americamysis bahia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES# NC0083321 Facility Hubert WTP Outfall 001 Project# N.q'L O County Onslow I Test Concentration(Acute Limit) 90% Dilution mL mL Total volume Samp.e was not aerated or treated unless otherw se noted on this form The samp a was warmed t, preparation: Sample Dilution water mL 25 0 2 1 0 C;n a warm water bath.Artdrcui sea sat was added to the sample to raise the sal my to 25 0 2 1 0 ppt The samp a was then diluted to the test concentration w th sat synthet:water 990 110 1100 tiFeeding Test Initiation or Termination Location Randomising Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst Incubator/Shelf Template it 0 24 li •Test organsms were fed n hold.ng 2 t_5 h.,ws pr or to test inmat en Test organ.,ms were n led d„r-g the re.t Chemical Analyses: •Analyst identified for each day,performed pH and dissolved oxygen measurements only.Temperature and salinity performed at the time of test initiation or termination by the analyst performing the toxicity test. Initial Final Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench sheets O Concentration and transcribed to this bench sheet. Analyst �� pHISUI %.-t,, 1'Cfa1 Chemical analyses: Dissolved oxygen(mg/L) 1.1 7 •7 Parameter Reporting limit Method number Meter Serial number II Control Salt SW °Salinity(ppt, 1q•- —L.4 '& pH 0.1 5.U. SM 4500-Ho B-2011 Accumet AR20 93312452 A 'Alkalinity(mg,l CaCO,) 1150 l Dissolved oxygen 1.0 mg/L SM 4500-0 G-2016 Y5I Model 52CE 180104324 'Temperature(c) ?1, 1—°1•lt Conductivity 14.9 µmhos/cm SM 2510 8-2011 Accumet AR20 93312452 pH(S U 7(1r(1 Salinity 1.0 ppt SM 2520 B-2011 Y51 PRO30 180104324 Dissolved oxygen(mg,L( , —I Alkalinity Alkalinity 5.0mgCaCO,/l SM 2320 8-2011 Accumet AR20 93312452 g Test / V Concentration 'Salinity(opt) 24,9 tS•O Total residual chlorine 0.1 mg/1 ORION 97.70-1977 Accumet A8250 92349123 'Temperature •C .-�r-.•w't p ( ) 11'17 W.) 'IAA Temperature 0.1°C SM 2550E-2010 Digital Thermometer ,NsA 1`�S lil100% pH(S.u) g.pb Test Organism Information: Ja't (salinity Dissolved oxygen(mg/L)Adlusted( 1.6 Organism Source: Aquatic Indicators,Inc. 'Salinity(ppt) 21.0 Batch(Al Batch Ab): 04-18-22 pH IS.0 I -1s \-k Age(1 to 5 days old): \-'L DA.ls 100% Dissolved oxygen(mg/1) �`•o Date organisms were born: 04-17-22 1200 to 1 'Salinity(ppt) S.9 O 04-18-22 1130 Conductivity(µmhos/cm) 10,01 Average transfer volume: <0.25 mL I 'Total residual chlorine(mg/L) ..Or t0 Transfer bowl information: pH(S u.)= %.-0 Temp.(°CI= Z.1•0•C Survival Data (number of living organisms): 1 Control Test Concentration Statistics: Hours Method \tS'�_ I N P Replicate Replicate s I A B C D E F G H t-stat or Rank N C, 0 10 10 10 10 10 10 10 10 I tailed Critical yJL Initiation I 7 9L 247� d a t— (0 ,o ro /0 3 3 1 if PASS or FAIL FN. Termination Mean survival: /007 Mean survival: '2-1.S 1. IComment codes: d=dead,u=unhealthy,s=stressed SOP AT41-Revision 5-Exhihit AT41.2 desi r j mac, IP • • 351 Depot Street Asheville,NC 28801 Phone: (828)350-9364 Fax: (828)350-9368 Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility Environmental Chemists,Inc. NPDFS" NC008332 I Pipe g 001 County Onslow Hubert WTP Purchase order Species Ansericantysis(Mysidopsis)Win Effluent dilution 90% Test type 24-hour Pass/Fail Acute Parameter code TAA3E Sample information: (to be completed by sample collector) Composite sample: Sample location 1.1 T 17 LT PFlvev, Start date y//9J'/J-:L Time: 0115 Volume collected for testing 4 L End date 4///y/,2 z. Time: O 9 3 e, Number of containers filled for testing Number of samples per hour 1 Method of transport to laboratory End,;real fe..r Chilled during collection') ye! Comments If chilled,specify temperature Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must he<6.0"C upon receipt at the lahorators. Sample custody: (to be completed by sample collector and facility personnel) Sample collected by: C4G16r1►►y t..laber ait ' 09'OS r,v,t s.N�,. D.0 and um. Relinquished by: Received by: Cale-, h �/tbor 444 y�'�z2 et) a rltq�^ GAY(l` ,►l�1 y 2� ' ) rn�t s,r",w" D.S ,dnn,. Inns ...�._.- \ /t��tn..� Relinquished byi Received by: Cowt,;c wt" y 11 y)zap FeCR`I- owl-1&-tt I'nnt S atum Due.M tune rnA Det,.na tam Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: Received at ETS by: F a�-tq. Ipc)00 owl Li-It �' �SJ+(N -1 IQ00 1'nv: Sirnnurt DO,and tune font Sir Mac and unw ^ Custody seals intact?: Sample temperature upon receipt at ETS("C): Vn Nt. Na usN O. C Samples received in good condition?: 1 L Y. 0 Total residual chlorine upon receipt at ETS: (DPD Presence Absense Indicator.MDL=0 10 mg/L) P"""t Ah'n' Tracking number: 441'1" .b ‘S 1-SStA Project number:(,0 20 Sample number:A20 Litg.Q I Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions,Inc. Source: Aquatic Indicators, Inc. I 1 I I 1 1 I I I 1 1 1 1 I I I I I 1 I 0.58 - - • 0.56 - Control Limits (± 2 Standard Deviations) • _ • 0.54 - • • 0.52 - - • • —•- - -' .. • • • 0.50 - • • • • - • • 0.48 - • • - V - - Y 0.46 - - tit) 0.44 - - 1 I I 1 1 1 1 1 1 1 I 1 1 1 1 1 I 1 1 1 0.65 IIIIIIIIIIIIIIIIIIII L G 0.60 - Warning Limits 00 • 41- 0.55 - • • • • • 0.50 - • • • •� • • • • • • • - • • 0.45 - ,..— _ . 0.40 - 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 I O L,01;��.Oti OA.06-O�.Oa 06.0%O�.1''0�.0'�09.1�10.05 l_01 1L-01�O�AA O LAB O L.16-O�.CO. �.1-OQ.OS ow ow oA.O1 OQ.15-LL Test date • 48-hour LCS0=median lethal concentration. An estimation of the potassium chloride concentration which is lethal to 50%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LC50 converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50± 2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LC50±SA.10 converted to anti-logarithmic values, SA 10= 10th percentile of CVs reported nationally by USEPA) xee.na •.w.w.a M nm sunnnw 22 --oq lCC PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Environmental Testing Solutions,Inc Fax: (828) 350-9368 May 16, 2022 Mr.Jay Baker Environmental Chemists, Inc. 6602 Windmill Way Wilmington, NC 28405 ETS Project Number: 16974 Test Start Date: 05-04-22 Facility Tested: Hubert WTP Enclosed are toxicity test results for samples received by Environmental Testing Solutions Inc. Parameter Result Test Procedure, Method Number Code PASS FAIL TGE3E Americamysis Pass/Fail Acute Toxicity Test X EPA-821-R-02-012, Method 2007.0 All toxicity testing results required as part of your permit must be entered on the Effluent Discharge Monitoring Form (MR-1) for the month in which it was performed, using the parameter code TGE3E. Additionally,the DMR Reporting Form AT-2 must be signed and e-mailed or mailed to the following address: ATForms.ATB(c�ncdenr.gov North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh, NC 27699-1621 Please call if you have any questions concerning these results. Sincerely, Jim umner Laboratory Supervisor North Carolina Certificate Numbers: Biological Analyses: 037,Drinking Water: 37786,Wastewater: 600 South Carolina Certificate Number: Clean Water Act: 99053-001 PO Box 7565 Asheville, NC 28802 Phone: (828) 350-9364 Fax: (828) 350-9368 Effluent Toxicity Report Form - Acute Pass/Fail Date: May 16, 2022 Facility: Environmental Chemists, Inc. NPDES 4: NC 0083321 Pipe#: 001 County: Onslow Hubert WTP Laboratory Performing Test: Environmental Testing Solutions, Inc., Certificate#037 Comments Signature of Operator in Responsible Charge(ORC): ORC Phone/E-mail: Project 4: 16974 Signature of Laboratory Supervisor: µ,"4, Sample#: 220504.21 e-Mail to: ATForms.ATB[cOncdenr.gov Or Mail Original to: North Carolina Division of Water Resources Water Sciences Section/Aquatic Toxicology Branch 1621 Mail Service Center Raleigh,NC 27699-1621 North Carolina Acute Pass/Fail Toxicity Test Collection Date: 05-02-22 Organism Tested Collection Time: 0730 Test Start Date: 05-04-22 Americamysis(Mysidopsis)bahia Sample/Type/Duration Grab Comp. Duration p Control 8.07 8.07 H(S.U.) X 24.5-h 4 Treatment 7.96 8.02 � X D C Alkalinity(mg CaCO3/L) 140 n Lu Salinity(Initial/Adjusted)(ppt) 24.7 5.8/24.4 Control 7.8 7.8 D.O. (mg/L) Total Residual Chlorine(mg/L) <0.10 Treatment 7.9 7.6 Sample Temp.at Receipt(°C) 3.0 Mortality Replicate Mean Mortality Treatment 1(Control) A B C D 0% 0% 0% 0% 0.0% Treatment 2(Exposure) A B C D Concentration 90% 70% 70% 90% 60% 72.5% Tested Note: If mean control mortality exceeds 10%,the test is considered invalid. Calculate using Arc-Sine Square t-Stat/ Rank Sum NC PASS Root transformed data. 1-Tailed Critical NC FAIL X If the absolute value of the calculated t is less than or equal to the absolute value of the tabular t,check PASS. If the absolute value of the calculated t is greater than the absolute value of the tabular t,check FAIL. If all vessels within each treatment have the same response but the treatment two response is greater than the control,check fail. DWR Report Form AT-2 Page 1of1 Acute Pass/Fail Whole Effluent Toxicity Test, Species: Americamysis bohia EPA-821-R-02-012, Method 2007.0 Client Environmental Chemists, Inc. NPDES# NC0083321 Facility Hubert WTP Outfall 001 Project# `tocrv-\ County Onslow 0 Test Concentration(Acute Limit) 90% Dilution mL mL Total volume Sample was not aerated or treated unless otherwise noted on this form.The sample was warmed to preparation: Sample Dilution water mL 25.0 i 1.0°C in a warm water bath.Artificial sea salt was added to the sample to raise the salinity to 25.0 i 1.0 ppt.The sample was then diluted to the test concentration with salt synthetic water. 990 110 1100 Feeding Test Initiation or Termination Location Randomizing Hours Date Sample Number Salt SW Batch Time Analyst Time Analyst Incubator/Shelf Template ° • tI° OS oa It o i 20 >>1.A y* tE qeuvu3 1'-°S q.zt cr1 ,.., u S 2termi4 t t•LS K 'Test organisms were fed in holding 2 to 5 hours prior to test Initiation.Test organisms were not fed during the test. Chemical Analyses: •Analyst ident lied for each day,performed pH and dissolved oxygen measurements only.Temperature and salinity Performed at the time of test initiation or termination by the analyst performing the toxicity test Initial Final Alkalinity and total residual chlorine performed by the analysts identified on the test specific bench sheets Concentration Analyst V VJ /`� ` ,(,( - and transcribed to this bench sheet. pH(s.u.) C 6.0 / Chemical analyses: Dissolved oxygen(mg/L) Parameter Reporting limit Method number Meter Serial number Control 2a �.: Salt SW 'Salinity(ppt) tA•' pH 0.1 5.U. 5M 4500-Hc B-2011 Accumet AR 93312452 1 'aril•9 *Alkalinity(mg/L CaCD,) 1.1 o Dissolved oxygen 1.0 mg/L 5M 4500.0 G-2016 Y5I Model 52CE 180104324 'Temperature(°c) ZS•ei 15.3 Conductivity 14.9pmhos/cm SM 2510 8-2011 Accumet AR20 93312452 pH(S.U.) '7 9''L 6a( 2 Salinity 1.0 ppt 5M 25208-2011 YSI PRO30 180104324 3� W Dissolved oxygen(mg/L) / V ()•(p Alkalinity 5.0 mg CaCOs/L SM 2320 B-2011 Accumet AR20 93312452 Test Concentration *Salinity(ppt) IA_r .LA Total residual chlorine 0.1 mg/L ORION 97-70-1977 Accumet AB2S0 92349123 'Temperature(°C) o •'1 Temperature 156.t. 1S .O P 0.1°C SM2550E-2010 Digital Thermometer 13e64gtrs 100% pH(s.u.) /t—f Test Organism Information: (Salinity Dissolved oxygen(mg/L) Adjusted) 95,0 Organism Source: Aquatic Indicators,Inc. 'Salinity(ppt) -t..k,1 Batch(AI Batch Ab): 05-02-22 pH(s.u.) 7-1 Age(1 to 5 days old): ' - 1 b A-I S Dissolved oxygen(mg/L) l Date organisms were born: O 100% l 05-01-22 1200 to 'Salinity(opt) J t 8 05-02-22 1130 Conductivity(pmhos/cm) 1°{00 Average transfer volume: <0.25mL 'Total residual chlorine(mg/L) L ► Transfer bowl Information:�. i OPH(S.U.)= S.I` Temp.(°C)= 1.3,,A.G Survival Data (number of living organisms): a Control Test Concentration Statistics: Hours Method v t SdAI 11Ji Replicate Replicate A B C D E F G H t-stat or Rank N L 0 10 10 10 10 10 10 10 10 1-tailed Critical Initiation 14 24 t O (0 I() (6 314k t9dl '4`4 PASS or FAIL FAt L Termination Mean survival: (CO. Mean survival: Zl, S 7- Comment codes: d=dead,u=unhealthy,s=stressed SOP AT41-Revision 5-Exhibit AT41.2 • • 351 Depot Street • crf Asheville,NC 28801 Phone: (828)350-9364 Fax: (828)350-9368 per` yJ Environmental Testing Solutions,Inc. Whole Effluent Toxicity Chain-of-Custody Form Facility Environmental Chemists,Inc. NPDES N NC0083321 Pipe n 001 County Onslow Hubert WTP Purchase order Species Antericainpsis(Mpsidopsis)bahia Effluent dilution 90% Test type 24-hour Pass/Fail Acute Parameter code TAA3E Sample information: (to be completed by sample collector) Composite sample: Sample location \ven Start date 5/a/...1.- Time U le 3 Volume collected for testing q End date 5/3/a a Time 0 7 10 Number of containers tilled for testing 1 Number of samples per hour f Method of transport to laboratory Errs, 4'04lie✓-- Chilled during collection" \/(? s Comments If chilled,specify temperature i r Triple rinse sample container with sample before filling. Completely fill the sample container with no air space. Pack the sample container completely in ice. The sample must be 6.0"( upon receipt at the laboratory. Sample custody: (to be c.-mpleted by sample collector and fae.dits persr.,nnel Sample collected by: onyl C n 1.,, 1-r-14/e bar Qvt�—, -s/J)a Pmi ,.,t, Deb Relinquished by: Received b): y,� � Da� gdlee%H.w0bal � stO i1/iA Tout BeASt � vier, :� 2 Pam �....i.i. De uW tom �,. Apub.e bti'- I1+b w vine Relinquished by: Received by: 1S�l� `krf � 032z Pam 'C! neb.nv vine t.,r• 5y,.:me Due.nJ unb Sample receipt information: (to be completed by ETS personnel) Relinquished to ETS by: r Received of ETS by' Fceltt 1'nm ,arts,r 192mc putute Deb and nine Custody seals intact?: EJ EJ Sample temperature upon receipt at ETS("C): Not -CY., weal 3.� Samples received in good condition?: h 1 lli-----�..�--�ti Total residual chlorine upon receipt at ETS: r, 1-7 `��� 3s 1 �SL� (DPD Presence Absense Indicator MIX-0 10 mg/L) Tracking number: 11 Sample number: R Project number:1(4qm { O37•2—I Comments: Americamysis (Mysidopsis) bahia Acute Reference Toxicant Control Chart Environmental Testing Solutions,Inc. Source: Aquatic Indicators, Inc. I I 1 ( I I I I I I I I I 1 I I 1 I I I 0.58 — — • 0.56 - Control Limits (± 2 Standard Deviations) • • 0.54 — • • • — 0.52 — — • 0.50 — • • • • • •• • • — • • .� 0.48 — • • — u - - 0.46 — — J - - b- 0.44 — — G I 1 1 1 I I I I 1 I I I I I I I I I I I J 0.65 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 I 0 0.60 — Warning Limits s 00 • 0.55 — • • • • • • 0.50 — • • • • I • • • • • • • • 0.45 — — 0.40 — — 1 I I I I I I I I I I l I I l I 1 I I I 03 d oek06�S of O6 0$0�,13 O�03 o9.lp 10Ras- �.0 601 0�OQ�ti0$�L S6 Q3 0$031ti�,os ot.os�a 0l�.19 OS 03-� Test date • 48-hour LC =median lethal concentration. An estimation of the potassium chloride concentration so which is lethal to S0%of the test organisms in 48-hours(calculated using ToxCalc). Central Tendency(mean logarithmic LCso converted to anti-logarithmic values) Control Limits (mean logarithmic LC50±2 standard deviations converted to anti-logarithmic values) Laboratory Warning Limits(mean logarithmic LC50±2 coefficent of variations converted to anti-logarithmic values) USEPA Warning Limits (mean logarithmic LCso±SA to converted to anti-logarithmic values, 5A.10=10th percentile of CVs reported nationally by USEPA) tIleol*ed wrs APPENDIX E Page 1 of 3 Sample# 202200255 Field ID Hubert Water Treatment Plant Lagoon Host Ponds; Lakes; impounded waters Received Date 5/4/2022 DIAGNOSTIC REPORT County Onslow Contact: Submitter: James Arnold Plant and Pest Diagnostic Clinic ONWASA Plant and Pest Diagnostic Clinic 228 Georgetown Rd. 511 Westinghouse Road JACKSONVILLE NC 28540 Pendleton SC 29670 Phone Fax 864-646-2178 Phone Fax Email Email 910-340-9214 jarnold@onwasa.com ppclnc@clemson.edu Diagnosis and Recommendations Host/Habitat Ponds;Lakes;impounded waters(Aquatic habitat) i List of Diagnosis/ID(s) Filamentous green algae(Mougeotia sp./spp.) Filamentous green algae(Spirogyra;Oedogonium;Cladophora sp./spp.) Filamentous green algae(Spirogyra;Oedogonium;Cladophora sp./spp.) Fragilia sp. Eunotia sp. Preliminary Report Report from Dr. John Hains: This is an interesting sample. It originated in a water supply pond for the Hubert Water Treatment Plant, ONWASA, Jacksonville, North Carolina. Their note mentioned that this is a moderate infestation but expect it to grow as temperatures warm. This suggests that there is a history of recurrence for this infestation. Fish are present, it is not used for irrigation, but animals drink the water. They also noted the presence of geese which may suggest nutrient enrichment. The mass of filamentous algae contains several filamentous genera such as Mougeotia, Oedogonium, and an unbranched form that I believe is Cladophora. All of these are in the Chlorophyceae (green algae). Cladophora is the dominant component of this infestation and it is well-known for luxuriant growths such as tit this. That said, it does not produce toxins although its decomposition may contribute to oxygen consumption "A and anoxia. It is a common nuisance algae and in abundance it likely indicates abundant nutrients. ' Plant and Pest Diagnostic Clinic Diagnosed By: Plant and Pest Diagnostic Clinic William Cory Heaton(heaton2@clemson.edu),John Hains 511 Westinghouse Road (jhains@clemson.edu) Pendleton SC 29670 Completed Date:5/23/2022 Telephone:864-646-2133 Page 2 of 3 At high magnification I also noted the presence of abundant diatoms, single-celled algae that have silica cell walls. These usually indicate decent water quality and the genera that I identified rarely, if ever,cause any problems. The notorious'rock snot',Didymosphenia, is not present in this sample. The diatoms were dominated by Fragilaria,Eunotia and similar genera. Dr. Heaton, I believe, may be able to advise on biological controls for this infestation if other measures are not allowed for water supplies. I also add that if this infestation of green algae is eliminated without also addressing the conditions that contribute to its growth,that habitat will remain available for other types that may be even less desirable to replace it. Final Report Control recommendations by Dr. Cory Heaton: Planktonic Algae Control There are numerous herbicides on the market that can be used to control planktonic algae and cyanobacteria blooms. The most commonly used algaecides contain chelated copper or sodium carbonate peroxyhydrate as the active ingredient. Copper algaecides should not be used in waters with hardness below 50 ppm. Common copper algaecide brand names include Cutrine-Plus,K-Tea, Captain, etc. Common sodium carbonate peroxyhydrate algaecide brand names are Phycomycin, Green Clean,and Pak 27. Application rates for copper algaecides range from 0.6 to 3.4 gallons per acre foot. The peroxide products are an excellent option for cyanobacteria species. Application rates for sodium carbonate peroxyhydrate algaecides range from 3-170 pounds per acre foot. Application rates vary between brands purchased so exact recommendations will be based on the product you select to use. All application information can be found on the label of the algaecide selected. Please note that application rates are in acre feet or water acres. Acre feet equal the surface acres multiplied by the average depth. It is very important that you do not over apply copper algaecides as copper can be toxic to fish. Planktonic algae typically can be controlled using the lowest recommended rate of the algaecide selected. Dissolved oxygen depletion can occur following herbicide applications to aquatic weeds. It is recommended to aerate pond waters for several nights following an herbicide application. Additionally,ponds with high density weed populations should be treated in sections 10-14 days apart. Filamentous Algae Control Mechanical Removal Filamentous algae can be manually removed from the pond via rake or seine. This can be labor intensive,and require multiple cleanups throughout the growing season. Biological Control Triploid grass carp rarely consume filamentous algae, and as such offer very little control. Numerous species m of tilapia consume algae,and are often stocked for algae control in South Carolina. Tilapia are tropical fish 4 and are not capable of surviving normal winter conditions in SC waters. Typical stocking rates of tilapia for algae control are 200-400 per acre. Stockings should be made at the higher rate if the pond has largemouth bass. N Chemical Control Plant and Pest Diagnostic Clinic Diagnosed By: Plant and Pest Diagnostic Clinic William Cory Heaton(heaton2@clemson.edu),John Hains 511 Westinghouse Road (jhains@clemson.edu) Pendleton SC 29670 Completed Date:5/23/2022 Telephone:864-646-2133 Page 3 of 3 Copper algaecides are the most commonly used products for algae control in private ponds. They come as copper sulfates or chelated coppers. Chelated coppers are readily available at most agricultural supply businesses. Common brand names include Cutrine-Plus, Captain, K-Tea, etc. Copper is known to be toxic to fish. It is extremely important that you follow the directions on the product label to ensure that your fish are not harmed. Label will provide information on water alkalinity and hardness levels required to make copper applications. Sodium carbonate peroxyhydrate is another algaecide that is commonly used in private ponds. This is a peroxide based algaecide that is not toxic to fish. This product is commonly marketed as Green Clean, Pak 27, and Phycomycin. Dissolved oxygen is a major concern when controlling aquatic weeds in ponds. When plants die following herbicide applications dissolved oxygen is needed for decomposition. When a pond needs herbicide applications it is recommended that herbicide applications be done to sections of the pond at 10-14 day intervals. This will reduce the potential of fish loss due to low dissolved oxygen. Ponds should be aerated for several days following herbicide applications if possible. to B U Plant and Pest Diagnostic Clinic Diagnosed By: Plant and Pest Diagnostic Clinic William Cory Heaton(heaton2@clemson.edu),John Hains 511 Westinghouse Road (jhains@clemson.edu) Pendleton SC 29670 Completed Date:5/23/2022 Telephone:864-646-2133 This diagnosis or identification is based only on the sample and its accompanying information.Because of this,the findings may not apply to the entire planting or habitat. Use all recommended pesticides according to label directions,following all precautions and restrictions. APPENDIX F BT SOLUTIONS, LLC 24-HOUR ACUTE FORM EPA 821-R-02-012 CLIENT: D N i, "1S A iwC 1°0 % SAMPLE LOCATON: /Jhe r1/ tJ a c /red-rne Pla r) TEST START(DATErrIME): -3/!°2/2 �qoD TEST END(DATE/TIME): _ SAMPLE UrAGE SAMPLE ID COLLECTION WHEN USED DATE/TIME 03a.22a - 1 3J9/.2a OBOO THROUGHOUT EOUGHOUTESTT EN TEST ORGANISM: k Americamvsis bahia AGE: .3 QI FEEDING: kI i.1j1 IcL2d/ 14-)-]em+a ( 3 Po?/o2.2 /103 DATE/TIME BIRTH: J ORGANISM TEST SOURCE: 'Marti-1 CD #OF ORGANISMS PER REPLICATE: yi5 LAB WATER BATCH: �'f(e) (`), cQ 12 o2 - as Test Solution Volume:>_ I OD mL Test Chamber Volume: 200 mL Dilution Volume: mt Test Termination:Control>90%survival 5 DAY DATE TIME Aerated at Start? How Long? INITIALS START 3pa/aa 19o0 n r rt 24 H R 3 f 2 3/a 2 19(2,0 E-v._DT NOTATION KEY *=Missing Organism RESULTS Fu)T ala202 48-HOUR L . METHOD OF D [NATION:TOXCALC 5.0 TRIMMED SPEARMAN KARBER 95%CONFDENCE LIMITS: COMMENTS: BTS-020 REV#0 Eff. Date: 03/01/2022 Page 1 of 4 Test ID ,L/t,) T f Date 91.2.2MA MORTALITY DATA: TREATMENT 0 H 0 H 0 H 0 H 24 H 24 H 24 H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) eon-601 ,Q . 5 9 -.c `}.(o a-1. 1 0 -g`1.9 6.(,c '}.O a 4 4 0 13 0 tin-treded 4 a50 8.a �.� �.5-.0 3 25 o 7.a t9.1 a5.� 50/ a Alo. Add. 1,4 aLl_a 8.0 8.4 5 1- 5- a5 t -1-. 5 6. S co. 8 1 oo /. a 5 a5.5 6. 3 '. S .262.3 5 ay 8 3.6 4_5 a 5.0 8 5 pNr� 4 251 $.(k 1.9 .2s aq8 -1. 8 IDS a5.5 80 /. 8 Ii Ae,0_4 1 R 6.(8 5 a 4 dq.7- g 6,9 a ,. S 3o •�. 6 3 AerceJ3 a a5. 5.(4, 7.62 .24- I 4 25. 2 1.8 1- 0 ,24. 0 ' o 6 5 Pete- r t a .2 1,.0 8. 430 0 o2 i/. (c 5 a 5. (0 3.(8 7.0 2 L Go 100 a 5 F l+e.acl i 4 .25-8 6.4 •1- 5 3 a s. 3- 1.5 "To Y. 8 F;acted 3. A .25.9 g.to -4-.5 .2 s 4 5 ;)5 4 -3-.9 6119 a 5 5 ic�o •t. 5 F Ikred ,1 a as 5 g.f, 4_ 5 a24- 5 a5.5 8.0 ep. 3 a4 So Q 4 C 18 l A as./ 8.5 3 5 Q 5.5 5 a5.5 �.9 (,. � .255 to o I. 5 BTS-020 REV#0 Eff. Date: 03/01/2022 Page 2 of 4 Test ID f-J W T F Date 0.2 MORTALITY DATA: TREATMENT 0H 0H 0H 0H 24 H 24 H 24H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) CIE 3 A. L1. 3 s 3.-4 as.l 4 - y3 S c' 7. 4 a7.0 801. Q Ct ,� c24.5 S.4- 1.5 a4. 2 1-1-3 Th9 1.° a`1_ 5. qv•l• a .2. EDTA 19 g.3 7.9 as o q a1. 3 8. 0 4. 1 025 3 go /. a La1A 3Q, A ail a 8 .2 7 9 a4_9 y Q 3 <3,0 -7o /. Q 3 EDTA 75 A w.24.� 8. i 7.9 a,i.S 3 ail 3 8. O 7-0 a5. 0 (00 3 [Do!< , A .24to 7.Io 7.9 .21_ S 3 .74 J 8 .O 1.0 .24 8 ./. 8 tj711 3ac A a5.0 it- 7.9 24- 3 3 1. & 024 `i t o 7. 8 3 K0. e.3A .25..2 S. 3 4.5 25.5 aL9 7. g -" at0 80 /. 3 ' 1 -T.9 12.5 A .24_I 8.3 8.0 .25 3 aq_9 7.9 0 at D -7n 'I 1kTh 25 A ail.a 8. 3 8.0 ail 8 4.9 c i'3 015. 9 r3 3 i(cxh,aSD A O246 8- 3 1.9 025.a 3 a4S 5 5. /55 6d 7 3 3 • FILL: L0 la' A a'+.I S 3 7. 9 . S.5 5 (24.6 -4. 9 5. a 5 .2 q o � h BTS-020 REV#0 Eff. Date:03/01/2022 Page 3 of 4 Test ID LJ T P Date 31a2a,,2_2_ MORTALITY DATA: TREATMENT 0H 0H 0H 0H 24 H 24 H 24 H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) Ae, ,b,161.-^k 4 .2 1- 8 . 3 7.4, as.io 0 12 I SI 0 3 a L. o O (3 0 r.I t, -4g7,13b.k a s 4.'-I 9.1 1.0 a 5.lv 0 .2 Li v g 0 3- 3 2 5-9 83 0 OS Ql.Ak A at 3 S.D -7-.1c .25.6 O '24 S' D 7- 3 a 5 f' D 8 0 BTS-020 REV#0 Elf. Date:03/01/2022 Page 2'of 4 4 BT SOLUTIONS, LLC 24-HOUR ACUTE FORM EPA 821-R-02-012 CLIENT: OKI u r lS1 IWC ,00 % SAMPLE LOCATON: 14k`3)or1� I�f0 Cam' Irec kY1?n 1� ()JQf n 1 TEST START(DATEITIME): �)19 -1 I(4° CO TEST END(DATE/rIME): y! I5 lad I idC,7 SAMPLE USAGE SAMPLE ID COLLECTION WHEN USED DATE/TIME 3 ( 14f5I 0�30 TEL NTIRE TIR000HO TEST TEST ORGANISM:Americamvsis bahia AGE: 2 , 0 FEEDING: . I4r1 Ic2 DATE/TIME BIRTH: N / I2'22 �1 ORGANISM TEST SOURCE: -0l(j" c` #OF ORGANISMS PER REPLICATE 10 LAB WATER BATCH: J(,�I (`Y) I,3,2e 5 Test Solution Volume:>_ (SOmL Test Chamber Volume: 2450 mL Dilution Volume: — mL Test Termination:Control>90%survival ✓ r DAY DATE TIME I Aerated at Start? How Long? j INITIALS START 441141,22 1(0 1,1 24 HR t-Fj is/ I l� C-1-01 NOTATION KEY * =Missing Organism RESULTS 48-II011R LC50. METHOD OF !NATION:TOXCALC 5.0 TRIMMED SI EARMAN KARBER 95%CONFDENCE LIMITS: COMMENTS: BTS-020 REV#0 Eff. Date: 03/01/2022 Page 1 of 4 Test ID JJu_`x, T ►L Date 4/i+Jaa MORTALITY DATA: TREATMENT 0H 0H 0H 0H 24 H 24H 24H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) 1, n,r,f-1 A 0Kilt s. ► o 1,2 0240 o -24.o 3 . 1b I. 4.07 Q _ 6j 8,14(.4 y4ptjay '7 un*ea- 4 aq_o s .a.► '7. a5:3 &Ll. l 1_a'a I.I a5 D Q 013 A a4,0 8.20 7.4 a1.4_ I S - .2 4.1 79L1 '7.3 a4.q f35 6 9 A (24,o 4.8`8 7.4 24. 3 3 a4. l }. 0 4.3 a 5-9 y 5 Floc Q _ Q Mc"-icdi aLt.t, 3.43 7.LI a4.3 a41 1-.9* 1.3 a5.0 3-0 here / 91t 1. `i .25. 1 oZ 024:0 -7.g5 3 a a5. 35 5 tkg 11 µ .24. 1 0. 1g IA a5._O 5 025 5 /. 75 7. a a5. 1 (, 5 F1'c a $ f%l feci 0 a,-1.0 S,3te 1. 7 a`1-1 8 .25*.ln "7.9 9-, /0.9_ a 41.3 1.5 , kiked 3 a of 3 $.19 3- 6 a4:c6 a5 S 7..q5 GA a5. 1 45 D �:l Iered ll A 0211-a 9.2O •: 2 4.to 8 255 . 6`j. to- 8 a 4. (Q S 019 ; A 014.o s.41-1 7.4 a4..( -4- .25 5 g.00 co-9 2 4. 1 5 6 g C i8 3 A 024-o V-53 7 1- P2L/.40 7 25,5 1.9ci col 21. 1 _ --- - to - - - BTS-020 REV#0 Eff. Date: 03/01/2022 Page 2 of 4 Test ID Date 4104 42-Z MORTALITY DATA: TREATMENT 0 H 0 H 0 H 0 H 24 H 24 H 24 H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) Cis l a a4.1- 1- 0216 LI 644,9,9 .ua 61. 2LI. 5 ElAim ; a a s .11 7.4, a3. l p .24 S•24- 12.9 .9LI- f a a ft&l n. 3 p ;N. (Q 9,12 714 a a.' ., a y. ( s. a4 6.. 3 .24. I o 6 O _ HAD-A_ 9 A a4 (d.19 1. 3 24.0 6 a4.© s .a3 o 4..0 0 8 o EDrA ,q A aL/.° , a 5,q a Ll. a 8.D4 6- 9 a 5.8 ( 5 rDTA 3g A 024.o ga3 1.s a5. 8 3 .24/. 1 Rol. a5.s _ 3 3 3 _ CDTA q5 A a'.D SAG `LI a 5 f 3 014.a S.06 To a 5. 3 D 3 �;sn_ --- .24.y ire EDT, isty A .3. 1.i o ?.9 a 5.5 3 a�. 5 g.©LI 1.0 Q 5,5 3 () _..) E V(,4 n - 3 EDTR 3oo A o2 gl. l 711 7.9 5 I ( a 41. la ' .8a .O Q5. I 15 C ckwe) (3 _ NaT<;s o 6.9 d 74.3 8.15 7.7 a 5-`8 S . .2.4. 3 7.9 5 (o_(o 5. 6 80 _ 6 8 I40-1,;, I2.s A d�t.� �.Ig -. g a `� 7 0?&1.3 7-967 (- a5.1 1-5 a _ 8 r .T a:o 25 A Li.D 93.19 1.1 a5.9 7 024. 3 7.98 66, a 5' 9 d 4 ' � BTS-020 REV#0 Eff. Date:03/01/2022 Page 3 of 4 Test ID Tl1-7 Date 41144 i-22 MORTALITY DATA: TREATMENT 0H 0H 0H 0H 24 H 24H 24 H 24 H 24 H %MORT TEMP pH DO SALINITY # TEMP pH DO SALINITY (°C) (su) (mg/L) (PPT) DEAD (°C) (su) (mg/L) (PPT) f1/4Sa,Th.a50 i 24.3 B-20 .9 ..5 4 a 4. 1 1.99 to a s.y 145 aj\i _ s aTh;o►o@ a •if `g Jo 1:1- 015-b - a . a 1.99 to 5-'8 40 a 1 0e►c_faw1 k a Az& S . 1I c{ 024.4 © I g.,25 ` •o a'4.5 r 2q+.7 ' t9 _ 3 ael ,o o a a4.- a.a14 To 224 . 3 8 1.1 io-hk A a4(0 '165 7. 14 .24 O ® 24.3 a�.l 8�18 �.�► 0 Cl-k ,•1364 A 24 3 g.r8 a a ail. I g.a3 7.i .2 '. 0 c� d sGI:4: �4_t -161 � . a 5. 1 to a4.D S. 13 7-0 5' 0 ��us}.Q.d A C`� 6 ID I BTS-020 REV#0 Eff. Date: 03/01/2022 Pagel of 4 MARINCO BIOASSAY LABORATORY The Aquatic Toxicology Specialists NELAP Certification#E84191 Shipment Record State of Florida Aquaculture Certificate Number AQ0668007 Shipping Date: 4/i 3 2ov t Ship to: >3 1 5 0/c,17 tons P.O. No: Species Quantity Age Brood/Lot Temp. pH Salinity Number (°C) (S.U:) (°/oo) Americamysis 500 2-1)A-14 HSZZO '// 7. 7 Z' bahia Menidia beryllina - Hardness mgl.L Cyprinella leedsi Pimephales promelas Ceriodaphnia dubia Daphnia magna YCT P. subcapitata Packed by: , Shipped Via: FLnoep-- Notes: Thank you for your order. 4569 Samuel Street•Sarasota,FL 34233•Tel:941-925-3594•Fax:941-922-3874•Web:www.biologylab.com Organism Shipment Record 2008 ver.3 11/17/2008 SHEALY CONSULTING, LLC N9 5058 SHEA . . CHAIN OF CUSTODY RECORD NAMING.Luc 343 W.Columbia Avenue• Batesburg-Leesville,SC 29006 Telephone No.(803)582-7996 Page of www.shealyconsulting.net Client Ct\i. 4 4 a 0 fvg Address 3 7..z /4-k.1 c.z_+ !> f v D City � Sta e Zip Code .. I.+VI/>e r✓ f e ' ` Preservaive I.Unpres. 5.HCL Project Name 2.NaOH/ZnA 6.Na.Thin. 14Ji3c-Z t- Ta • C. i` Y 3.H2504 7.NaOH Sampler Name j privi Phone# ‘1 . Igy Bottle Size: !6AL a HNO3 Preservative Codes: Sample ID/Description co,"pos're Shealy LabSam P P Or Sampler Start Sampler End Indicate number of containers in the boxes below. (Containers for each sample may be combinerd on one line.) crab Date Time Date Time =r 0,V wa SA it►.J 4-1-1 fop-. c :+-1 Sr c,-/n,'t t} ( 3 1. .a, .2 Z 3. 1r 2., ? .. 3 G,:.,I.,0S c •7 33 b gz,c) 03 2.�z.2 - I 1.Relinquished by Date Time 1 R-.: ed by Date Time •i'kvhf.S I 4,L .141 7_,-- __-- 1 3-Re-A.,-(2 i 35-/ I _ 2. 'shed b )' late Ti 2. •ived b _� q 4 Q c f -- 3 1 (/ QGu.t +'!�—I.S ltq I22- Tim1 (3 0 3.Reliaquished by 57: T©�u� 3.R d by 3 a112� Time t_ec t .� �, !!//�. �2 ek 0 / 0 9 0 4. Relinquished by Date Time 4. Re ved by Date Time ❑ Continuation of Custody on attached sheet 0 Received on ice(Circle) Yes No Ice Pack SC Receipt Temp 3.'IC DISTRIBUTION:WHITE-Return to laboratory with Sample(s);CANARY-Field/Client Copy Document Number:SCF-TS-248 Rev.3 Effective Date: 6/1/2017