A twelve-month protocol for reproducing, characterizing, and stress-testing the CuFe-PBA / COP aqueous battery chemistry at grid-relevant rates. Every measurement maps to an Emerson instrument.
This protocol governs the Phase 1 laboratory validation of an aqueous magnesium-ion battery based on the CuFe-PBA cathode / COP anode chemistry published by Chen et al. (Nature Communications, February 2026). The paper demonstrates 120,000+ cycles at 20 A/g with a 2.2 V full-cell voltage using a non-flammable, near-neutral pH electrolyte. Phase 1 answers the question the paper leaves open: does this chemistry survive at grid-relevant C-rates?
Reproduce the full-cell architecture using pre-purified battery-grade MgCl₂ (Nedmag, Netherlands). Characterize electrochemical performance at C/10, C/4, C/2, and 1C. Establish degradation curves, copper leach rates, and impedance evolution over 1,000+ cycles at each rate.
Develop a repeatable, instrumented process to purify industrial-grade MgCl₂ (Intrepid Potash, Carlsbad NM) to battery-grade (≥99.9%) using Emerson DeltaV and Rosemount sensors. Validate via ICP analysis against Nedmag baseline. Qualify domestic electrolyte for cell production.
| Parameter | Target | Kill Threshold | Instrument |
|---|---|---|---|
| Capacity retention at C/4, 1,000 cycles | >95% | <80% | NI HPS-17000 |
| Coulombic efficiency | >99.5% | <95% | NI HPS-17000 |
| Electrolyte pH stability | 4.91–7.02 | <4.0 or >8.0 | Rosemount 3900 |
| Copper leach rate | <5 ppm per 100 cycles | >50 ppm per 100 cycles | ICP-OES |
| Track B purity match | ≥99.9% | <99.5% | ICP-OES |
| Impedance growth (EIS) | <20% at 1,000 cycles | >50% | NI PXI |
The aqueous chemistry is intrinsically safer than lithium-ion (no flammable solvents, no thermal runaway). However, synthesis involves reagents that require standard chemical laboratory safety.
K₃[Fe(CN)₆] is stable and non-toxic under normal conditions. It must never contact strong acid (pH < 3). Acidification liberates hydrogen cyanide gas (HCN), which is lethal at >300 ppm. All ferricyanide work must occur in a fume hood with continuous airflow ≥100 fpm face velocity. Dedicated acid-free zone. Spill kit with sodium bicarbonate (NaHCO₃) immediately adjacent.
| Zone | Minimum PPE | Additional |
|---|---|---|
| Zone A — Electrolyte | Lab coat, safety glasses, nitrile gloves | Face shield when handling NaOH ≥1M |
| Zone B — Synthesis | Lab coat, splash goggles, nitrile gloves | N95 respirator when handling K₃[Fe(CN)₆] powder; fume hood mandatory |
| Zone C — Testing | Lab coat, safety glasses | Hearing protection near environmental chamber compressor |
| Gas | Sensor | Low Alarm | High Alarm | Action |
|---|---|---|---|---|
| H₂ | Rosemount 928 / 628-H₂ | 1,000 ppm | 2,500 ppm | LOW: investigate, increase ventilation. HIGH: evacuate Zone B, DeltaV SIS shuts down electrolysis. |
| HCN | Dedicated electrochemical | 2 ppm | 5 ppm | LOW: stop ferricyanide handling, verify acid segregation. HIGH: evacuate lab, initiate emergency protocol. |
| O₂ | Glovebox oxygen analyzer | >1 ppm | >5 ppm | Glovebox breach. Purge. Do not open antechamber until <0.5 ppm. |
The core measurement stack is Emerson hardware. Two supplementary instruments (EQCM and vapor pressure osmometer) are sourced from specialty vendors; all primary process control and electrochemical characterization runs on Emerson-manufactured equipment.
All reagents are commodity chemicals. No controlled substances, no conflict minerals, no export-restricted materials. Total Phase 1 materials cost: <$28,000.
Three reference diagrams for the Phase 1 team. The cell schematic defines the physical stack order. The voltage profile shows what a healthy charge/discharge curve looks like. The Nyquist plot shows what healthy impedance looks like and how degradation manifests.
Schematic representations. Actual impedance magnitudes will be determined during formation (Procedure F, Step 03).
Two parallel tracks (A: Nedmag-purified, B: domestic-purified) × two parallel concentrations (4.0M handling-optimized + saturated 5.8M paper-replication). Chen et al. characterizes the cell at saturated MgCl₂ (~5.8M at 25°C), with 1M and 3M tested for water-in-salt regime comparison. The proposal’s 4.0M handling-optimized concentration sits below precipitation-risk threshold and remains in the WIS regime (aw < 0.55). Phase 1 tests both side-by-side as a publishable Phase 1 deliverable: establish the optimal grid-scale concentration for industrial deployment. All target pH 6.5–7.5.
| Parameter | 4.0M (handling-optimized) | Saturated ≈5.8M (paper-replication) |
|---|---|---|
| Mass MgCl₂·6H₂O per 1 L H₂O | 813.2 g | ~1180 g (saturation limit) |
| Density @ 25°C | 1.290–1.300 g/mL | 1.355–1.370 g/mL |
| Conductivity @ 25°C | 180,000–220,000 µS/cm | ~250,000–310,000 µS/cm (decreases above 4M due to viscosity) |
| Water activity (aw) | 0.45–0.55 | 0.32–0.40 |
| Viscosity @ 25°C (cP) | ~9–12 | ~28–40 |
| Precipitation risk < 15°C | Low | Moderate — warm to 25°C before use |
| Cells in matrix | ~46 cells (Tracks A+B, all C-rates) | ~46 cells (Tracks A+B, all C-rates, paper-direct comparison) |
Why test both: (1) saturated reproduces Chen exactly — the calibration cell that says “our hands match the paper’s hands.” (2) 4.0M is the engineering candidate — lower viscosity means better ion transport at scale, easier industrial handling, and lower precipitation risk in cold climates. Phase 1 deliverable: a head-to-head cycle-life and round-trip-efficiency comparison at C/4 and C/2. The optimal grid-scale concentration becomes the answer the rest of the field will cite.
What Chen et al. used. Saturated MgCl₂ (~5.8M at 25°C) is the headline electrolyte in the published paper, with 1M and 3M tested for comparison (SI Figs. 13–14). The COP polymer family is Hex-TAPZ, Hex-DABZ, and Hex-TADD; Hex-TADD-COP is the headliner that delivers the 120,000-cycle result. Source supplier and reagent grade are not disclosed in the publicly accessible Supplementary Information; standard Chinese university convention is Aladdin, Macklin, or InnoChem analytical-reagent grade (≥99% MgCl₂·6H₂O hexahydrate). Phase 1 verifies this against the supplier’s certificate of analysis before using.
Track A — Nedmag (Netherlands), the safe baseline. Solution-mined from the Veendam deposit in eastern Netherlands. Reserves: estimated 1.5–2.0 billion tonnes MgCl₂-equivalent. Current production: ~440,000 tonnes/yr salt across the company’s product mix. At full Phase 3 scale (3–5% global stationary storage market capture), Emerson demand projects ~50,000–150,000 tonnes/yr electrolyte-grade salt. Nedmag reserves support >100 years at that rate. “Running out” is not a Phase 1–4 concern.
Track B — Intrepid Potash (Carlsbad, NM), the US security play. Industrial-grade MgCl₂ (90–98% purity) from existing US potash operations. Phase 1 Track B establishes the DeltaV purification protocol that lifts this to ≥99.9% (Nedmag-equivalent). Closes the geopolitical gap; eliminates Netherlands single-source dependency for US deployments.
Track C — Desalination brine, the inexhaustible source. Global desalination plants discharge ~142 million m³/day of MgCl₂/CaCl₂-rich brine, almost all dumped to ocean. Capturing 0.1% of this stream supplies Phase 4 demand perpetually. Track C economics depend on Phase 1 Track B purification protocol working at scale — which is why Track B is committed in Phase 1, not deferred.
Summary: Nedmag alone covers Phase 1–4 with multi-decade headroom. Track B closes the geopolitical gap. Track C makes the supply effectively infinite. Salt is not the constraint — getting it pure enough is the constraint, and that is exactly the engineering Emerson is built to do.
Coprecipitation of copper(II) sulfate and potassium ferricyanide to form the open-framework Prussian Blue Analogue Cu₂[Fe(CN)₆]. Room-temperature synthesis. No specialized atmosphere required (aqueous reaction).
Solvothermal condensation of the covalent organic polymer. The COP stores charge through reversible radical cation formation — no intercalation, no volume change, no cracking. The absence of structural deformation during cycling is the mechanism behind the published 120,000-cycle result.
Chen et al. characterizes three covalent organic polymer variants from a common hexaketone monomer (Hex):
Phase 1 prepares Hex-TADD-COP for the primary cell matrix (Track A). Hex-TAPZ and Hex-DABZ are synthesized in smaller batches as comparison sets for ranking degradation pathways under the same C-rate sweep. Naming the specific variant matters because peer reviewers will ask, and because process-IP downstream (electrode formulation, binder, current density windows) is polymer-specific.
Unlike intercalation anodes (graphite, Li₄Ti₅O₁₂), the Hex-COP family stores charge via reversible radical cation formation at C=N active sites along the polymer backbone. The backbone accepts and releases electrons without structural deformation. No expansion, no contraction — the degradation mechanism that limits every intercalation-based battery does not exist here.
Standard slurry casting on metallic current collectors. The composition ratio — 70:20:10 active material : carbon black : PVDF — follows the paper. Coating uniformity directly determines capacity uniformity and cycle life.
Electrode slurry viscosity is a Rosemount measurement. Coating thickness uniformity at scale maps directly to Afag linear motion systems for doctor blade or slot-die application. This procedure is where lab science meets manufacturing instrumentation.
Identical procedure (steps 01–05) with the following substitutions:
| Parameter | Cathode (CuFe-PBA) | Anode (COP) |
|---|---|---|
| Active material | CuFe-PBA powder | COP powder |
| Current collector | Ti foil, 25 µm | SS 316L foil, 25 µm |
| Loading target | 1.5–3.0 mg/cm² | 1.0–2.5 mg/cm² (capacity-matched) |
| Doctor blade gap | 200 µm | 150–200 µm (adjust for capacity balance) |
The anode capacity must be 10–20% excess vs. cathode (N/P ratio 1.1–1.2). If the cathode delivers more charge than the anode can accept, metallic Mg deposits on the polymer surface rather than inserting into the C=N framework — irreversible capacity loss and potential dendrite nucleation. Calculate theoretical capacity from published specific capacity values, weigh both electrodes, and select matched pairs before assembly.
Two formats: CR2032 coin cells for rapid screening and Swagelok cells for long-term cycling. All assembly in the argon glovebox (O₂ < 1 ppm, H₂O < 1 ppm). Note: The electrolyte is aqueous, but the glovebox protects the COP anode from ambient oxygen, which irreversibly oxidizes the radical cation sites. Electrodes enter the glovebox dry; the degassed electrolyte is introduced at the last step via micropipette. The water is controlled, not excluded.
Identical electrode/separator/electrolyte stack in a PTFE-body Swagelok union fitting. Benefits: easy disassembly for postmortem analysis, larger electrolyte volume (~1–2 mL), better seal for months-long cycling. Use 16 mm diameter electrodes with 18 mm GF/A separator.
Format: [TYPE]-[TRACK]-[BATCH]-[SEQ]
Example: SW-A-0301-04 = Swagelok, Track A electrolyte, March Batch 01, Cell #4
Example: CR-B-0602-11 = CR2032, Track B electrolyte, June Batch 02, Cell #11
| Purpose | Format | Qty | C-Rate | Track |
|---|---|---|---|---|
| Formation screening | CR2032 | 20 | C/10 | A |
| C-rate sweep | Swagelok | 12 | C/10, C/4, C/2, 1C (3 each) | A |
| Long-term cycling | Swagelok | 8 | C/4 (4), C/2 (4) | A |
| Temperature study | Swagelok | 8 | C/4 @ 0/25/40/55°C (2 each) | A |
| Track B qualification | Swagelok | 8 | C/4 (4), C/2 (4) | B |
| Electrolyte reuse test | Swagelok | 4 | C/4 | A→reuse |
| High-precision coulometry | Swagelok | 4 | C/4 (2), C/2 (2) | A |
| Self-discharge / calendar | Swagelok | 4 | C/4 charge, 72h rest | A |
| EQCM (in-situ mass) | EQCM cell | 4 | C/10 (slow, mass-resolved) | A |
| Postmortem reserve | CR2032 | 16 | Various | A |
| Total | 92 |
Slow initial cycling establishes a stable electrode/electrolyte interface. In aqueous systems there is no traditional SEI layer, but the first cycles activate the PBA framework and establish the COP radical cation equilibrium.
The central experiment. Four C-rates, each run to 1,000+ cycles. No group has published rate-dependent cycling data for this chemistry. These measurements determine whether the lab result translates to a grid product.
After 1,000 cycles at each rate, fit capacity vs. cycle number to both linear and power-law degradation models. Extrapolate to 80% capacity retention (industry-standard EOL for BESS). Compare extrapolated cycle life at C/4 against the 120,000 cycles demonstrated at 20 A/g. The ratio defines the practical-vs-laboratory performance discount factor — this single number determines commercial viability.
Every characterization technique below has a defined cadence, a target parameter, and an action threshold. The schedule is designed to catch degradation mechanisms before they become ambiguous.
| Technique | Instrument | Cadence | What It Reveals |
|---|---|---|---|
| EIS | NI PXI | Every 100 cycles | Charge transfer resistance evolution. Early warning for electrode degradation, electrolyte decomposition, or interface passivation. Rct growth >50% triggers investigation. |
| ICP-OES | ICP-OES | Every 500 cycles | Dissolved Cu, Fe, K, Mg, Ca in electrolyte. Quantifies cathode dissolution rate. Cu accumulation trajectory predicts remediation interval. |
| pH | Rosemount 3900 | Every 100 cycles | Electrolyte acidification/basification trend. Drift outside 4.91–7.02 range indicates uncontrolled side reactions. |
| Conductivity | Rosemount 228 | Every 500 cycles | Electrolyte concentration stability. Significant drift indicates water loss (evaporation from imperfect seal) or salt consumption. |
| dQ/dV Analysis | NI HPS-17000 | Every 100 cycles | Differential capacity plots reveal changes in redox peak positions and intensities. Phase changes, new side reactions, and loss of active material all have distinct dQ/dV signatures. |
| XRD (postmortem) | External lab | M6, M12 | Crystal structure of cycled CuFe-PBA cathode. Confirms framework integrity, detects amorphization or phase transitions. Compared to as-synthesized baseline. |
| SEM/EDX (postmortem) | External lab | M6, M12 | Electrode morphology, particle cracking, copper deposition patterns, binder distribution. EDX maps element distribution across the electrode cross-section. |
| Rate Capability Check | NI HPS-17000 | Every 500 cycles | 5-cycle sweep at C/10 to verify recoverable capacity hasn’t degraded independently of rate effects. |
| GITT | NI HPS-17000 | M1, M3, M6, M9, M12 | Galvanostatic Intermittent Titration Technique. 10-min current pulse at C/10, 60-min OCV relaxation, repeat across full SOC range. Yields Mg²⁺ apparent diffusion coefficient (Dapp) in both electrodes as a function of SOC and cycle age. The rate-limiting step at C/4 vs. 20 A/g is almost certainly diffusion — GITT quantifies it directly. |
| High-Precision Coulometry | NI HPS-17000 (HPC mode) | Continuous (dedicated cells) | Coulombic efficiency measured to ≥4 decimal places (e.g., 99.95% vs. 99.99%). At 120,000 cycles, even 0.01% parasitic loss per cycle compounds to 100% capacity loss at cycle ~7,000. Two dedicated cells at C/4 and C/2 run HPC continuously. This is the Dahn method — the only way to predict multi-decade lifetime from 12 months of data. |
| Self-Discharge / Calendar Aging | NI HPS-17000 | M3, M6, M9, M12 | Charge to 100% SOC, rest at OCV for 72 hours (25°C), measure residual capacity by full discharge. Grid batteries idle at partial SOC for hours between dispatch cycles. Self-discharge >5%/month at 25°C is a red flag for parasitic side reactions consuming Mg²⁺ or water. |
| Water Activity (aw) | Vapor pressure osmometer | Every batch + M3, M6 | Confirms the “water-in-salt” regime. At 4.0M MgCl₂, expected aw ≈ 0.45–0.55. If aw > 0.7, free water is available to split at 1.23 V and the expanded stability window claim does not hold. Measured on fresh and postcycling electrolyte to detect dilution from water ingress. |
| Raman Spectroscopy | External lab (confocal Raman) | M3, M6, M12 | Ex-situ Raman on electrolyte: the O–H stretching region (3,000–3,700 cm⁻¹) shifts when water molecules coordinate to Mg²⁺ vs. remaining as free water. Tracks WIS regime stability over time. Also detects CN– stretching (~2,100 cm⁻¹) from any ferricyanide leaching from the cathode framework. |
ICP copper data is the single most important degradation metric. Plot Cu concentration (ppm) vs. cycle number for each C-rate. Extrapolate to determine the cycle count at which Cu exceeds the remediation trigger threshold (target: define this threshold during Phase 1). If Cu leach rate at C/4 is <5 ppm per 100 cycles, remediation intervals of 6+ months are feasible. If >50 ppm per 100 cycles, the copper contamination problem may dominate the system economics.
This data directly feeds the Rosemount continuous monitoring + electrowinning remediation loop described in the full proposal.
Minimum n = 3 cells per condition (C-rate × temperature × electrolyte track). All capacity retention and coulombic efficiency values reported as mean ± standard deviation. Batch-to-batch reproducibility validated by requiring <10% coefficient of variation (CV) in initial discharge capacity across ≥3 synthesis batches before committing cells to long-term cycling. If CV exceeds 10%, investigate synthesis parameters before proceeding.
Go/no-go gate criteria apply to the worst-performing cell in the group, not the mean. A single outlier with capacity retention <80% triggers investigation even if the group mean is >95%. The conservative interpretation protects Phase 2 from survivorship bias.
Phase 1 commits to a byproduct philosophy: every output stream is either a saleable product, a regenerable consumable, or processed on-site to non-toxic discharge. Zero stream leaves the lab in a form that creates downstream liability. The lab pays its own electric bill (load bank), recovers its own copper, and ships out a higher purity electrolyte than it received.
| Output | Yield & Purity | Recovery Path |
|---|---|---|
| Recovered copper From cycled-cell cathode leaching | 5–15 g per 100 cycled cells. Dendritic powder, ≥99.5% purity after electrowinning. | emew or ElectraMet bench rig in Zone A. Output sold to scrap refiner at LME spot (~$13–14/kg as of June 2026); at Phase 2 scale, routed back to Emerson sensor manufacturing as raw stock. |
| Cycled-cell electrodes Postmortem residuals | Sub-gram Cu/Fe per cell, but stoichiometrically valuable. | Phase 1: archive intact for forensic XPS/SEM/EDS. Phase 2: acid leach + electrowinning recovers active material. Zero landfill. |
| Stream | Regeneration | Net Consumption |
|---|---|---|
| Spent zeolite Track B Ca/Sr removal column | NaCl brine elution — in-place, no removal from skid. | ≥50 regeneration cycles per bed. End-of-life: ground zeolite is non-toxic mineral filler, sold to construction-aggregate market. |
| NMP, DMSO, DMF Synthesis / electrode wash solvents | Small distillation still in Zone B. Recovery: NMP ~95%, DMSO ~92%, DMF ~90%. | ~5–10% of nominal usage leaves as residue. Phase 2 goal: replace NMP with water-based binders (CMC/SBR, proven in Li-ion industry) to eliminate the stream entirely. |
| Input | Treatment | Discharge |
|---|---|---|
| Ferricyanide wash water | NaOCl oxidation in-line. CN⁻ → cyanate (CN⁻O). | Verified <1 ppm CN⁻ before drain. Cyanate is non-toxic at the expected concentration; municipal-permit compliant. |
| Copper-contaminated electrolyte | Inline ICP. <25 ppm Cu → routed to recovery loop above. >25 ppm Cu → electrowinning recovers ~95% before discharge. | Discharge stream: <1 ppm Cu, pH 6.5–7.5, mineral salt water. Compliant with municipal wastewater permits in all 50 states. |
NMP → eliminated (water-based binder substitution).
DMSO / DMF → 99% recovery via second-pass distillation.
Copper → 100% recovered, sold or reused.
Cells → recovered to active material at scale.
By Phase 2, the only outputs that leave the building are electricity (load bank discharge to Shell Space LEDs), recovered copper (sold), and mineral salt water (compliant discharge). Nothing else.
Stage 1 capex now itemized in companion proposal v14: $24–48K Zero-Discharge Capital line covers solvent distillation still (Zone B), NaOCl in-line dosing system (Zone A), bench-scale electrowinning rig (emew or ElectraMet contract), recovery-loop plumbing & DeltaV integration, and a Phase 2 lifecycle-assessment scope study. Phase 2 commits to publishing a peer-reviewed LCA demonstrating the closed loop.
The Phase 1 lab has a measurable, finite electricity demand that we should size honestly before we promise a load-bank offset. Equipment-by-equipment continuous and intermittent loads, the operating-hour assumptions, and the projected cost are below.
| Equipment | Continuous (kW) | Peak (kW) | Hours/day | kWh/day (avg) |
|---|---|---|---|---|
| NI HPS-17000 cycler (cycling load) | 5 | 150 | 6–8 (active) | 120–240 |
| Glovebox (Ar circulation, gas purification, lighting) | 3–4 | 5 | 24 | 72–96 |
| Environmental chamber (-40 to +85°C, intermittent) | 0.5 | 4 | 12 (avg) | 12–30 |
| HVAC + fume-hood makeup air (lab allocation, MN climate) | 10–15 | 18 | 24 | 240–360 |
| Vacuum oven, ICP-OES, EQCM (intermittent) | 0.5 | 5 | 4–6 (avg) | 12–25 |
| Solvent still + electrowinning rig (recovery loop, intermittent) | 0.2 | 5 | 4 (avg) | 12–20 |
| Lighting + DeltaV controllers + computers | 3–4 | 5 | 24 | 72–96 |
| Daily total (mixed duty) | ~25 | ~80–100 | — | 540–870 |
After build-out, the lab’s steady-state electricity is approximately 200–320 MWh/year at $15K–$28K/year. Load bank discharge is the primary offset in Phase 1 (returns lighting and base load to Shell Space). At Phase 2 scale, the load bank ties into the building electrical sub-panel; a 10 MWh facility-scale aqueous BESS at 80% round-trip efficiency would offset roughly half of annual lab consumption while serving as the demonstration unit. The lab does not pay for its own electricity at Phase 1 scale; it does at Phase 2 and beyond.
Convert industrial-grade MgCl₂ from Intrepid Potash (~95–97% purity) to battery-grade (≥99.9%) using the DeltaV-controlled purification skid. This process, once validated, becomes Product 6.
| Stage | Input | Purity | Cost ($/ton) |
|---|---|---|---|
| Raw feedstock | Intrepid Potash | ~95–97% | $200–600 |
| After precipitation + IX | Stage 3 output | ~99.5% | +$400–600 processing |
| After recrystallization | Stage 4 output | ≥99.9% | +$400–900 processing |
| Battery-grade total | ≥99.9% | $1,000–2,100 | |
| Nedmag imported | Netherlands | ≥99.9% | $1,500–3,000 |
Four checkpoints. What earns the next quarter of funding, and what kills the project.
Track A: CuFe-PBA cathode synthesized via coprecipitation, characterized (XRD, TGA, ICP, BET). COP anode synthesized via solvothermal route, characterized (FTIR, TGA, BET). First prismatic cells built with Nedmag electrolyte. Initial cycling at C/10 and C/4 underway on NI HPS-17000. DeltaV skid commissioned for Track B. Formation data on ≥20 coin cells.
| PASS | Cells cycle without catastrophic failure. CE >98% post-formation. pH within 4.91–7.02. Reproducible synthesis (≥3 batches, <10% capacity variance). |
| KILL | No cell survives 50 cycles. CE <90%. pH excursion >2 units. Synthesis irreproducible. |
Track A: EIS impedance data reveals degradation trajectory. Copper accumulation rate measured via ICP at 500 and 1,000 cycles. Coulombic efficiency trend established. dQ/dV analysis shows whether redox peaks are shifting. Rate capability check confirms recoverable capacity. Track B: first purification runs complete, ICP on purified product.
| PASS | Capacity retention >95% at 1,000 cycles (C/4). Cu leach rate supports remediation interval >6 months. EIS impedance growth <20%. CE >99.5%. |
| CONDITIONAL | Retention 80–95%. Cu leach 5–50 ppm/100 cycles. Continue with modified protocol and monthly reviews. |
| KILL | Retention <80% at 1,000 cycles. Cu >50 ppm/100 cycles. Impedance growth >50%. Chemistry does not scale to grid rates. |
Track B: ICP analysis compares domestically purified MgCl₂ against Nedmag spec across all measured impurities. If purity matches (≥99.9%, all impurities within 5% of Nedmag levels), cells switch to domestic electrolyte for remaining cycling. Purification process recipe documented for Product 6 development. Parallel: Track A cells at 2,000–4,000+ cycles depending on rate.
| PASS | Track B purity ≥99.9%. Cell performance on domestic electrolyte matches Nedmag baseline within 5%. Purification process documented and reproducible (≥3 batches). |
| CONDITIONAL | Purity 99.5–99.9%. Performance gap 5–15%. Additional purification step required (second recrystallization or activated carbon polish). |
| KILL (Track B only) | Cannot reach 99.5% purity. Performance gap >15%. Track B abandoned; continue Track A with imported Nedmag. Product 6 thesis not viable for Intrepid Potash feedstock. |
Everything on paper. Comprehensive dataset: cycle life projection at C/4 and C/2, copper remediation plan with economics, electrolyte reuse data, energy efficiency at each rate, domestic supply chain validation, temperature sensitivity map, electrode manufacturing reproducibility. Phase 2 decision made with data, not projections.
Phase 1 dataset + Phase 2 recommendation: fund it, modify it, or stop. The dataset includes: ≥3,000 cycles at C/2 with full characterization, degradation model with EOL projection, copper management protocol, domestic electrolyte qualification status, Bill of Materials update with real costs, and preliminary cell design for Phase 2 scale-up.
• Rosemount 228 conductivity (1 Hz)
• Rosemount 3900 pH/ORP (1 Hz)
• Rosemount 372 dissolved O₂ (0.1 Hz)
• Rosemount 928 H₂ gas (1 Hz)
• Micro Motion ELITE density (1 Hz)
• Fisher valve positions (1 Hz)
• Skid temperatures, pressures (1 Hz)
All continuous data logged to DeltaV historian with 1-year retention minimum.
• HPS-17000 cycling data (1 Hz per cell)
• EIS Nyquist/Bode plots (per session)
• ICP-OES elemental analysis (per sample)
• XRD diffractograms (per postmortem)
• SEM/EDX images (per postmortem)
• Electrode mass/thickness logs
• Batch synthesis records
EECOMOBILITY handles automated analysis. Manual entries in structured lab notebook (electronic).
| Frequency | Audience | Content |
|---|---|---|
| Weekly | Lab team | Cycling status dashboard (EECOMOBILITY), anomaly flags, equipment status, upcoming characterization |
| Monthly | Project sponsor | Capacity retention trends, copper accumulation curve, Track B progress, budget vs. actual, risk register update |
| Quarterly (M3, M6, M9, M12) | Executive / Go/No-Go committee | Comprehensive milestone report with gate criteria assessment, go/no-go recommendation, Phase 2 implications |
The published paper (Chen et al.) places the fundamental chemistry in the public domain. Emerson’s IP position derives from process know-how, not formula exclusivity: NI test protocols for cycling and degradation characterization, the copper remediation loop (Rosemount monitoring + electrowinning recovery), the DeltaV purification recipe, and aqueous-specific BMS algorithms for Zitara. All lab notebooks, synthesis records, and characterization data are Emerson trade secrets. External publications require executive approval.