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Pipe Scale Analyses for Cct Evaluation

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Pipe Scale Analyses for Cct Evaluation PIPE SCALE ANALYSES FOR CCT EVALUATION EPA REGION 5 LCR-OCCT WORKGROUP AUGUST 12, 2020 1 What is a Lead Service Line (LSL) pipe scale? • The combination of lead corrosion products and deposited materials found inside a LSL • Crystalline lead minerals • Deposited materials • Represents decades of reactions and changes in water quality/treatment 2 Why analyze LSLs? • To evaluate the state of corrosion control treatment (CCT) and understand lead release • To predict impacts of potential changes to CCT or other water treatment processes • To address shortcomings in the ability of theoretical models to predict the lead minerals forming in the field 3 Why analyze LSLs? • When present, LSLs are the largest source of lead to drinking water • Many decades out from removing all LSLs in the United States • Systems need to know by what mechanism lead release is being controlled 4 Lead minerals contain a lot of lead… 5 Considerations • Due to the complex nature of many LSL scales there are several practical and technical considerations to take into account • This presentation will focus on: • How to sample scale from LSLs • LSL scale analysis • Powder X-ray diffraction • Scanning electron microscopy/energy dispersive spectroscopy • Case study illustrations 6 Visual Characterization • Detailed description and Outer documentation of the scale Middle • texture, color, physical Inner characteristics etc. • “Macro” and microphotography Drinking Water • Designation of scale layers Lead Pipe Wall 7 Scale Layers Depending on treatment history and distribution system nuances Can be simple… L1 (Pb(II) carbonates) L2 (PbO - litharge) Or complex… L1 (amorphous Mn) L4 (PbO2 - plattnerite) L2 (amorphous Fe) L5 (lead phosphate) L3 (amorphous Si,Al) L6 (PbO - litharge) 8 Sampling by layer • Once the layers are defined the process of carefully subsampling the identified layers can begin • Can be time consuming, L1 depending on complexity of the scale L2 • In some cases may not be able to separate very thin or very L3 friable materials L4 Experience has taught that there can be distinct differences in the mineralogy of the layers, these nuances are lost when the scale is sampled as a whole 9 Resulting Material • Separated layers are then individually crushed and passed through a 75 µm sieve • One of the drawbacks of subsampling layers will be a low yield (~200 mg or less in some cases) • Some LSLs will provide plenty of material for certain layers whereas other layers can be difficult to obtain enough sample 10 ORD’s main components of scale analysis Analyses performed on individual layers: Destructive / Sample amount Analytical Technique Information Nondestructive needed Mineralogy of As little as 10 mg Powder X-ray Diffraction (XRD) crystalline Nondestructive (more is better) material X-ray Fluorescence (XRF) 200 mg Elemental Total Carbon/Total Sulfur (TC/TS) Destructive 50 mg composition Total Inorganic Carbon (TIC) 10-20 mg Scanning Electron Microscopy Images and spatial (SEM) / distribution of -NA- -NA- Energy Dispersive Spectroscopy elements (EDS) 11 Powder XRD Powder top-loaded onto silicon holder • Non-destructive method • Ability to analyze small amounts of material • Provides information Amyl acetate slurry regarding the crystalline onto quartz holder and (to some extent) poorly-crystalline components of the analyzed material 12 Cautions and Caveats • Contamination/Disturbances Trench Sediment Lead Shavings Cable Tooling 13 More Cautions and Caveats • Peak overlaps • Pipe scales are rarely composed of a single mineral phase • Auto-ID feature in pattern fitting software should be used with caution • Some practical knowledge of expected (and improbable) minerals in a drinking water environment is useful 14 Some XRD Pattern Complications Outer layer of ~10μm thick scale • Multiple phases • Peak overlaps • Sediment and lead • Pb phosphates rarely exactly fit database Outer layer (L1) Pipe scale Inner layer (L2) Lead pipe wall Lead pipe wall 15 Crystalline vs. Amorphous 16 SEM/EDS Analysis • Preservation of in-situ layer relationships from a representative undisturbed section of the LSL • Cross-sectional view • Useful for understanding complex layering 17 Cross Section equipment 18 Cross Section Preparation EDS WDS SEM Chamber 19 Elemental Maps are Useful for General Spatial Relationships BSD Epoxy L1 L1 L2 L2 L2 L3 Lead Pipe Wall EDS results from a spectrum taken over an XRF results from subsampling the individual entire area layers Element Weight % Element L1 L2 L3 Al 0.37 Al 1.4 0.8 0.3 Mn 2.05 Mn 7.4 2.7 0.2 Sn 1.05 Sn 2.8 3.1 1.4 Pb 78 Pb 58.6 71.3 83.620 SEM/EDS Interaction Volume 21 Caution Required When Evaluating SEM/EDS Results Common output for SEM/EDS analysis EDS Spectra Elemental Maps Al 0.6 wt% by XRF However, to truly interpret the Si elemental maps the 2.52 wt% associated spectrum by XRF needs to be evaluated Pb 93 wt% by XRF While Al appears across the entire map and at a comparable brightness to that of Pb and Si this cannot be interpreted as the elements are present in equal concentrations to one another 22 Case Study Illustrations • How can scale analysis inform decisions? • Diagnostic/Forensic • Track Results/Changes • Predictive/Preemptive 23 Diagnostic/Forensic Case Study 1: Washington, DC • Experienced LCR exceedances after switching disinfectants in the year 2000, chlorine to monochloramine • Added orthophosphate starting in August 2004 • LSLs from after the switch to monochloramine and after the addition of orthophosphate were analyzed 24 Scale Analysis Revealed… After ~ 15 months of 3- PO4 treatment Discontinuity surface P, Ca, O, and Al enrichment Orthophosphate was bypassing the relict Pb(IV) plattnerite layer at the scale water interface and was instead being incorporated into the lower scale layers 25 Washington, DC XRD Lead phosphate 26 Diagnostic/Forensic Case Study 2: Halifax, NS History of CCT changes • 1980’s – 1999: Lake Lamont Treatment Facility • orthophosphate at 1 mg/L and 1.5-2.0 mg/L during annual flushing/line cleaning • 1999: Lake Major Water Supply Plant brought on-line • 1999-2000: pH/alk CCT -- pH 7.6, alkalinity 19 mg/L as CaCO3 • 2001-2002: pH/alk CCT -- pH 7.8, alkalinity 32 mg/L as CaCO3 • 2002-2005: pH/alk CCT – pH 7.0-7.4, alkalinity 8 mg/l as CaCO3 • 2005: phosphate CCT using 75:25 ortho/poly blends – pH 7.4, phosphate dose at 1.5 mg/L, 2 mg/L during annual system flush. LSLs harvested in 2011 to evaluate why CCT was not lowering Pb levels as much as expected 27 Scale Analysis L3 L4 Revealed… • Thick Fe/Mn layer • Minimal development of lead phosphate • Leadhillite/susannite – not commonly found in Pb pipe scales L1 L2 Compound/Formula Layer 1 Layer 2 Layer 3 Layer 4 Poorly crystalline Fe & Mn ++++ Hydrocerussite (Pb3(CO3)2(OH)2) ++ +++ ++++ +++ Leadhillite/Susannite (Pb4(CO3)2(SO4) (OH)2) + ++++ +++ + Hydroxypyromorphite (Pb5(PO4)3OH) + + ++ ++ Litharge (PbO) ND ND ND ++++ 28 Phosphate tied up by Mn/Fe deposit L1 (thin – Mn-rich layer) L1 (thick – w/ Mn and Fe sublayers) L2/L3 L4 Element (wt%) Layer C O Al Si Ca Mn Fe Pb Zn P S L1 1.84 26.00 3.26 1.93 1.30 8.48 11.85 38.94 1.52 3.31 0.09 L2 3.02 10.10 0.88 0.57 0.31 0.20 1.56 81.87 0.20 0.62 1.05 L3 2.95 8.53 0.28 0.20 0.16 0.03 0.19 87.11 0.06 0.50 0.70 1 Tracking Changes Case Study 1: Fall River, MA • LCR exceedances from 1992-2006 • Due to aging infrastructure there was a minimal chlorine residual within the DS and residual was almost completely depleted within storage tanks • This resulted in a Total Coliform Rule Violation in 2001 • After increasing the chlorine residual there was a Stage 2 Disinfection By-products violation in 2013 • As part of their LSL replacement program, EPA analyzed LSLs from the system annually beginning in 2001 29 30 2001-2013 XRD Evidence Blue boxes show pattern features for hydrocerussite Red dashed boxes show pattern features for plattnerite 31 Scale Analysis Revealed… • A mix of lead phases governing lead release within the system (Pb(II) and Pb(IV)) • Pb(IV) formation accelerated as a result of water treatment plant improvements (2005) and was found to remain stable into 2006 • LSLs from 2013 show a regrowth of hydrocerussite which indicates deteriorating conditions for maintaining stable Pb(IV) and low Pb release 32 Tracking Changes Case Study 2: Providence, RI • Surface water system (Scituate Reservoir): pH 10.3, alkalinity ~15 mg/L as CaCO3, hardness ~42 mg/L as CaCO3 • Fall 2005 – Spring 2013: pH lowered to 9.7 to optimize dissolved Pb (based theoretical model understanding) • 90% Pb levels increased from 10-15 μg/L to 20-30 μg/L • Pb on iron particulates • LSLs extracted and sent to EPA beginning in 2006 (50+ pipes to date) • Testing orthophosphate CCT • Pipe loop: 2014 - 2016 • Partial system test: 01/2018 – present • Dose: 3 mg/L as PO4 33 Scale Analysis Revealed… • Crystalline calcium phosphate phase(s) precipitated on surface of pre-existing lead corrosion scales • Partial conversion of pre-existing hydrocerussite/plumbonacrite scale to calcium-substituted hydroxypyromorphite (Cax,Pb5-x)(PO4)3OH Pipe Loop Partial System Test 34 BSD Epoxy L1 L2 L3a Lead Pipe Wall 35 Something unexpected • PbO2 developed on parts of 3 of 4 LSLs harvested from the partial system test zone • Occurs only on areas underlain by PbO (litharge) • Previously observed on only 2 pipes of 50 harvested between 2006 and 2014 36 Predictive Case Study: Newport, RI • Surface water system, pH ~8.3, free chlorine, pH/alkalinity CCT, very reactive organic material • Due to DBP issues (particularly in consecutive systems), was contemplating
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