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. 2022 Dec 8;10(1):21–26. doi: 10.1021/acs.estlett.2c00581

Seasonal Fluctuations in Nitrate Levels Can Trigger Lead Solder Corrosion Problems in Drinking Water

Kathryn G Lopez †,*, Jinghua Xiao ‡, Christopher Crockett ‡, Christian Lytle †, Haley Grubbs †, Marc Edwards †
PMCID: PMC9835880  PMID: 36643386

Abstract

graphic file with name ez2c00581_0004.jpg

After a utility switched its source water from ground to surface water in 2017, first draw water lead levels spiked due to increased lead solder corrosion that could not be explained by existing knowledge. When lead release was not adequately reduced with a 90:10 orthophosphate/polyphosphate corrosion inhibitor blend or even high levels of 100% orthophosphate, an in-depth investigation of possible causes revealed a strong correlation between 90th percentile lead and seasonal fluctuations in surface water nitrate levels. Complementary bench-scale studies that tested new copper coupons with lead solder and harvested pipes from a worst case home verified a strong relationship between nitrate and elevated lead. Lead release in the presence of nitrate became increasingly erratic with time, resulting in the spalling of large lead solder particulates up to 7 mm in length into the water. Lead levels were occasionally >1000 ppb in homes and >100000 ppb in the bench experiments with harvested pipe. Orthophosphate was unable to sufficiently reduce lead levels below the action level during periods with high nitrate levels in the bench studies. Water utilities and regulators should proactively consider possible unintended consequences of higher nitrate levels on lead release when changing source waters or during seasonal runoff events.

Keywords: contamination, drinking water, electrochemistry, particulate matter, phosphates

Introduction

Lead solder is a major source of lead in drinking water causing U.S. Environmental Protection Agency (EPA) Lead and Copper Rule (LCR) exceedances. Lead release due to galvanic corrosion of lead solder and copper can be extremely sensitive to water chemistry parameters such as the chloride-to-sulfate mass ratio (CSMR), alkalinity, pH, and corrosion inhibitors in a manner that is different from that of either leaded brass or lead pipe.1−8

Nitrate is not currently considered in EPA lead corrosion control guidance.9 Prior research on nitrate focused mainly on its relatively insignificant effects on lead solubility for brass and lead pipe.10 Only one prior laboratory study showed that increasing the nitrate concentration from 0 to 2.5 mg/L in synthetic water could increase lead release from new solder by 194 times and trigger the erratic detachment of particulate lead.11,12

The EPA National Primary Drinking Water Standards currently permit ≤10 mg/L of nitrate in public water systems due to its potential effects on public health, including blue baby syndrome. In areas where nitrate is monitored on an annual basis, acute spikes above 2.5 mg/L due to seasonal fertilizer application and runoff events may not be detected. Meanwhile, nitrate levels are increasing in many U.S. surface waters and groundwaters despite mitigation efforts.13−15

This research explored the effects of seasonal nitrate spikes on lead solder corrosion via complementary studies with new galvanic copper–solder simulated joints, harvested copper plumbing samples, and intensive monthly field sampling in consumer homes. It also explored orthophosphate’s ability to control nitrate-induced solder corrosion. The work was conducted in response to unanticipated high water lead problems arising after a utility switched from a low-nitrate groundwater to a surface water with higher seasonal nitrate levels.

Materials and Methods

Utility Field Data

Beginning in May 2019, monthly compliance LCR samples were collected from 26–72 homes (SI Table 1). Water samples were collected from fire hydrants in the distribution system to monitor parameters such as chloride, nitrate, and sulfate levels. The utility serves a population of <10000, and there are no known lead service lines in the system.

Lead Solder Coupon Study

New galvanic coupons were prepared by melting 1 ± 0.05 g of 50:50 lead–tin solder along the 1 in. length of a 3/8 in. diameter copper coupling and placed in 125 mL glass jars. After being conditioned for a week in the original groundwater (SI Table 2), the coupons were exposed to one of three water conditions (n = 15) to simulate the source water change: control (surface water), control with nitrate (added as sodium nitrate), or control with nitrate and 1 mg/L orthophosphate as P. The surface water was shipped weekly by the utility for use in experiments (SI Table 2). Water was changed three times per week using a static collect-and-fill protocol, and weekly composite samples were analyzed using standard methods with 2% HNO3 for at least 24 h to dissolve metals.

Harvested Pipe Study

In May 2021, 13 copper pipes were extracted from a home in the affected community with persistent and erratic elevated lead levels. The pipes were filled with water and capped with rubber stoppers. For 1 week, they were conditioned with shipped surface water augmented with 1 mg/L orthophosphate as P, with water changed daily using a dump-and-fill method. Afterward, the pipes were grouped into two categories: those with no visible solder joints (n = 8) and those with visible solder joints (n = 5). Water changes were conducted three times per week. After 49 days, 7.4 ± 0.5 mg/L NO3-N was added to three of five pipes with visible solder and four of eight pipes without visible solder to simulate a nitrate spike. All pipes continued to receive 1 mg/L orthophosphate. Weekly composite samples were collected from each pipe and analyzed using standard methods. In some cases, 20% HNO3 and heating at 50 °C for 24 h were necessary to help dissolve the large particulates containing tin.16

Statistical Analysis

Statistical analysis of the data included multivariate regressions and pooled analyses of variance (ANOVAs) using lead, nitrate, and CSMR as parameters (SI Tables 3–6). All statistics were compiled in R (version 4.1.1) using an α value of 0.05.

Results and Discussion

Utility Field Data

Ninetieth Percentile Lead Correlated with Nitrate before the Addition of a Phosphoric Acid Inhibitor

Before the utility switched to surface water from groundwater in 2017, an expert desktop study did not anticipate that any problems with lead corrosion would occur according to the existing understanding.17 Within a year of the switch, first draw lead levels at some locations increased above the 15 ppb EPA LCR action level. The highest 90th percentile lead result over a 6 month regulatory monitoring period was 131 ppb in the first half of 2019, and the highest 90th percentile monthly result was 230 ppb in July 2019 (Figure 1). Occasionally, semirandom spikes of lead of >1000 ppb were detected in first draw samples of homes.

Figure 1.

Figure 1

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Utility monthly 90th percentile lead data before and after the switch from groundwater to surface water alongside surface water nitrate. The time periods during which the 90:10 ortho/polyphosphate blend and 100% orthophosphate were used are noted. The EPA LCR 15 ppb action level is included for reference.

Lead peaked between spring and early summer each year, corresponding with seasonal spikes in surface water nitrate levels up to 7.2 mg/L NO3-N in June 2021 (Figure 1). At other times, nitrate levels were generally <2.6 mg/L NO3-N. Fertilizer application and runoff are suspected causes of the spikes because the utility is located in a midwestern U.S. state where this is a known problem.18 After periods of high nitrate levels, inspection of aerators indicated that more large lead particulates were spalling off of home plumbing, which could dramatically increase water lead levels but also worsen correlations with nitrate due to the semirandom nature of particle release (SI Figure 1). Prior to the addition of a phosphoric acid inhibitor to the system in April 2020, an approximately half-month lag was observed between increasing source water nitrate levels and 90th percentile lead levels, which might imply a required exposure time for nitrate to affect lead monitoring data (Figure 1). Multiple regression analyses for this period used nitrate data paired with 90th percentile lead data shifted backward by a lag time (SI Table 3a). Lead was significantly correlated with nitrate (r2 = 0.46; p = 3.3 × 10–2) and not CSMR (p = 0.37), and a much stronger relationship between lead and nitrate (r2 = 0.79; p = 3.4 × 10–3) was obtained if the outlier lead spike that occurred in January 2020 was omitted from the model. CSMR, which was typically below the 0.58 CSMR corrosion trigger threshold, was not significantly correlated with nitrate [p = 0.12 (SI Figure 2)].8 Without accounting for a lag, the correlation between nitrate and lead decreased markedly [r2 = 0.27; p = 0.22 (SI Table 3a)].

Phosphoric Acid and Low-Nitrate Water Temporarily Reduced Lead Release

After the switch to phosphoric acid had been made, monthly 90th percentile lead samples temporarily decreased below the LCR action level. Phosphate was believed to be sufficiently controlling lead corrosion, although it was later discovered that source water nitrate levels also decreased to <2 mg/L NO3-N when the inhibitor was changed. Even after the phosphate dose was increased from ∼3 to 5.5 mg/L PO4 in November 2020, lead levels again increased above the action level along with an increasing nitrate level in spring 2021. While phosphate was in the system, the previously observed lag between nitrate and 90th percentile lead disappeared. With the smaller phosphate dose, 90th percentile lead data still correlated with nitrate (r2 = 0.79; p = 8.3 × 10–2) but not CSMR (p = 0.70). After the phosphate dose increased, neither nitrate (r2 = 0.56; p = 0.93) nor CSMR (p = 0.26) was strongly correlated with 90th percentile lead. According to the correlation, every 1 mg/L increase in nitrate corresponded with a 38 ppb increase in 90th percentile lead in homes (r2 = 0.70) before dosing phosphoric acid, which decreased to 32 ppb lead/mg/L of nitrate (r2 = 0.78) after the application of the smaller phosphate dose and decreased to 5 ppb lead/mg/L of nitrate (r2 = 0.42) after the application of the larger phosphate dose (SI Table 3b,c). These changes and the gradual decrease in lead spikes during high nitrate periods suggest that phosphate and time were gradually weakening the effect of nitrate. However, there may be a nitrate corrosion threshold above which phosphate offers only partial control. At ≤1.8 mg/L NO3-N, it was still strongly correlated with lead (r2 = 0.95; p = 1.1 × 10–2), and at >1.8 mg/L nitrate, it was no longer significantly correlated with lead [r2 = 0.63; p = 0.15 (SI Table 3a)]. This is possibly due to the semirandom release of lead particles described previously.

Lead Solder Coupon Study

Lead Release from New Leaded Solder Correlated with Ambient Nitrate Levels

In the first 124 days of the coupon study, surface water CSMR levels ranged from 0.42 to 1.0 and nitrate levels ranged from 0.45 to 7.8 mg/L NO3-N. During this period, the lead release from the control coupons was significantly correlated with both nitrate [r2 = 0.76; p < 2 × 10–16 (Figure 2 and SI Table 4a)] and CSMR [p = 4.49 × 10–2 (SI Figure 3)]. As the ambient nitrate level increased, the observed frequency and size (generally <2 mm) of the particles released increased. To differentiate between the effects of high CSMR and high nitrate levels, a side experiment using new lead solder coupons showed that lead release was roughly 2 times greater when coupons were exposed to a high CSMR level of of 1 plus an additional 5 mg/L nitrate compared to the control with only high CSMR [n = 5; p = 6.4 × 10–6 (pooled ANOVA) (SI Figure 4 and SI Table 5a,b)]. This suggests a synergistic effect of nitrate and CSMR on lead release and is consistent with a previous study that found that substituting nitrate for chloride in water while maintaining the same conductivity released 32 times more lead from solder.11

Figure 2.

Figure 2

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Lead release over time for all three coupon study conditions (control, with 5 mg/L NO3-N, and with 5 mg/L NO3-N and 1 mg/L orthophosphate as P) alongside ambient surface water nitrate. Error bars represent 95% confidence intervals. n = 15 through day 103, and thereafter, five coupons were randomly selected from each group to remain in the study. After day 103, composite samples were collected. After day 166, coupons in the orthophosphate condition were repurposed for another study.

High-Nitrate Treatment Triggered Large, Erratic Particulate Lead Release from New Lead Solder

Lead release from coupons exposed to an extra 5 mg/L nitrate was significantly correlated with both nitrate (r2 = 0.53; p = 3.5 × 10–5) and CSMR (p = 0.014) and generally produced ≈1–3 times higher lead levels than the control group through day 124. The size and frequency of particulate lead release were similar to those of the control group. After day 124, supplemented nitrate was increased to 8 mg/L, and within 2 weeks, very large black or silver solder particles up to 4–6 mm in length began erratically sloughing off of the coupons. A single particle of this size could contribute ≤54% of lead in a weekly coupon composite sample and double the normal relative standard deviation (RSD) for the 15 replicates (SI Figure 5). A lead spike occurred around day 194 for the control and high-nitrate conditions that coincided with the release of large (∼4 mm in length) particles, which is likely due to prolonged exposure to ambient nitrate above a previously suggested corrosion threshold of 2.5 mg/L NO3-N and the higher CSMR level.11 Following the increase in the nitrate level, lead release for the high-nitrate condition was no longer significantly correlated with nitrate (r2 = 0.056; p = 0.54) or CSMR (p = 0.84), whereas the lead release for the control condition that had fewer large lead particulates was still correlated with nitrate (r2 = 0.76). Throughout the study, lead release for the high-nitrate condition was significantly greater than that of the control [p = 5.9 × 10–5 (pooled ANOVA) (SI Table 4c,d)]. Thus, this may be a case in which extremely high lead levels resulting from erratic particulate release masked the correlation observed under the control condition with lower lead release. The effect of increased nitrate on lead release and evolution of erratic particulate lead release with time was replicated in a side experiment that exposed new lead solder to various levels of nitrate treatment [n = 5 (SI Table 5c,d and SI Figure 6)].

Orthophosphate May Not Sufficiently Control Lead Release in High-Nitrate Waters

Lead levels from coupons exposed to supplemented nitrate waters (1800 ppb on average) were significantly reduced with orthophosphate treatment [1450 ppb on average; p = 2.6 × 10–4 (pooled ANOVA) (SI Table 4c,d)]. On average, 93% of phosphate dosed was recovered in the effluent and >75% of this phosphate was soluble. For the first 124 days, lead release from coupons treated with orthophosphate was significantly correlated with CSMR (p = 1.95 × 10–6; r2 = 0.45) but not with nitrate (p = 0.39). After the nitrate increase on day 124, lead release was not significantly correlated with either nitrate or CSMR (r2 = 0.74; p = 0.15 or 0.50, respectively). Lead release from the orthophosphate condition was not significantly different than the control [p = 0.93 (pooled ANOVA)]. This suggests that orthophosphate may weaken the relationship between lead and nitrate but cannot reduce lead levels below the action level when nitrate spikes.

Without considering the effect of CSMR, every 1 mg/L increase in nitrate in the first 124 days resulted in 312 ppb lead for the control condition, 286 ppb lead for the high-nitrate condition, and 254 ppb lead for the orthophosphate condition (SI Table 4b). The increasingly erratic release of lead particulates in the high-nitrate condition can help explain why the slope for that condition was smaller than the control even though lead release was generally higher for the high-nitrate condition. For all of these conditions, >50% of the lead was in particulate form in the early phases of the study when soluble lead would be most important (SI Figure 7).

Harvested Pipe Study

High Nitrate Triggered Significant Lead Release from Harvested Pipes with Solder

The pipes were harvested from a home that frequently tested with the worst lead levels in the sampling pool. For 56 days, the harvested pipes were reacclimated to the surface water with a phosphate inhibitor to which they had been exposed for 12 months before extraction. During this time, lead release from all pipes declined along with surface water nitrate and CSMR (Figure 3a and SI Figure 8). Lead release from the harvested pipes with visible external solder was 23 times greater on average [p = 9.55 × 10–5 (SI Table 6a)] than from pipes from the same home without visible solder. Approximately 99% of this lead was particulate (SI Figure 9). Lead release among the pipes with visible solder was also more variable [141–24400 ppb; day 56 RSD = 155% (SI Figure 10 and SI Table 7)] than pipes without visible solder (12–879 ppb; day 56 RSD = 66%). This variability from one harvested pipe to another is attributed to differences in workmanship and the amount of solder in contact with water (SI Figure 11). To account for this extreme variability, each pipe with visible solder was considered individually (SI Table 6b and SI Figure 12). Within the first 56 days, three of the five visible solder pipes were significantly correlated with nitrate (p = 0.016–0.045), and of those, only one was also significantly correlated with CSMR (p = 0.049). Lead and tin were correlated in four of five pipes with visible exterior solder (p = 3 × 10–4 to 0.02) and seven of eight pipes without visible exterior solder [p = 8.4 × 10–15 to 0.005 (SI Table 6c)].

Figure 3.

Figure 3

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(a) Average lead release from the four pipe groups vs ambient nitrate. Error bars represent 95% confidence intervals. (b) Example of a lead particle approximately 7 mm in length released from a harvested pipe with visible solder.

On day 56, select pipes began receiving extra nitrate while the surface water nitrate level was <1.5 mg/L NO3-N and the CSMR level was relatively constant around 0.50. Pipes that received additional nitrate but had no visible solder saw no significant change in lead release (p = 0.35). Lead release levels between the two groups of pipes with visible solder were not statistically different before the change in nitrate treatment [p = 0.21 (pooled ANOVA) (SI Table 6d,e)] but were statistically different thereafter [p = 9.53 × 10–4 (SI Table 6f,g)]. The average lead release from the pipes with visible solder receiving additional nitrate increased by 1–3 orders of magnitude, and this was sustained through the end of the study. In contrast, lead levels for the pipes with visible solder not receiving additional nitrate remained within their original range. It is important to note that the correlations between lead and nitrate worsened for two of the three solder pipes receiving additional nitrate (r2 = 0.16–0.24; p = 0.65–0.83), which corresponded with the semirandom release of large lead particles. This effect on the correlations is expected given that the lead solder particles released at higher nitrate levels were often ∼4 mm in length [the largest was 7 mm (Figure 3b)] and could contribute ≤163000 ppb of lead to samples individually. These lead levels are at least 1 order of magnitude greater than observed in our prior work in Greenville, NC, and Flint, MI, where lead from solder reached 6000 ppb. Another point of reference is a newly constructed research facility studied by the EPA in 1995 where lead release from solder reached 1400 ppb.12,19,20

Comparison of New Lead Solder to Harvested Pipe

Lead release from the harvested pipes with visible solder was often 1–2 orders of magnitude greater than that of the coupons. There has been speculation that these extremely high levels of lead in the pipes can be attributed to (1) the longer duration of high-nitrate treatment because the pipes were exposed to the new surface water for more than 3 years before extraction, (2) more concentrated samples because the average pipe volume was 92 mL while coupons were in 125 mL jars, and (3) a large cathode:anode surface area ratio (a galvanic corrosion driving force) that is roughly 6:1 for the coupons and was probably much greater for the real pipes (SI Figure 13).21

Implications

Existing industry knowledge and EPA corrosion control guidance did not predict the major increase in lead release from solder that was observed after the source water switch.9 This is worrisome because many utilities are changing from groundwater to surface water due to sustainability regulations and other water quality concerns. Without the utility’s monthly sampling campaign, the relationship between the lead spikes and nitrate in this case study might have gone undetected, because LCR sampling often occurs in summer months when nitrate levels are low. Similarly, some utilities monitor nitrate only once a year, which might not capture important acute fluctuations. For example, the 2016 Consumer Confidence Report for a nearby city using the same surface water reported a single low nitrate measurement of 1.5 mg/L NO3-N.22 Water utilities and regulators should proactively consider these issues to prevent similar unexpected spikes in lead from occurring elsewhere. Additional research on the mechanism of nitrate-induced corrosion is needed to better understand and control this problem when it occurs.

Acknowledgments

The first author was partially supported by a NASEM Ford Fellowship and a Via Fellowship. The experimental work was supported by funding from Aqua America, Spring Point Partners LLC, and a grant from the EPA “Untapping the Crowd” Consumer Detection and Control of Lead in Drinking Water” (8399375). The opinions expressed in this report are those of the author(s) and do not necessarily reflect the views of Aqua America, Spring Point Partners LLC, or the EPA. Undergraduate students Brenda Velasco, Daisy Yates, Helen Salko, Nicole Paz-Jimenez, Torrey Schwab, and Trevor Stephens assisted with the laboratory work presented herein, and Dr. Jeffrey Parks assisted with weekly lead analysis.

Supporting Information Available

The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.estlett.2c00581.

  • Experimental details and two side studies (PDF)

The authors declare no competing financial interest.

Supplementary Material

ez2c00581_si_001.pdf (925.5KB, pdf)

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Associated Data

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Supplementary Materials

ez2c00581_si_001.pdf (925.5KB, pdf)

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