Six roles, three zones, twelve emergency procedures, a written Chemical Hygiene Plan, a 30-year service schedule, data recording standards, and a supply chain runbook. The manual the Shakopee Phase 1 lab runs on, and the procedure base for field deployments through 2056.
Who this manual is for, what it covers, how to read it, and the document-control regime that governs every revision.
Two audiences:
The six Phase 1 employees — PhD electrochemist (lead), Chemical Hygiene Officer, instrument tech, lab tech, half-time program manager, 0.2 FTE data engineer.
The Phase 2–4 field maintenance staff — service crews keeping deployed aqueous Mg-ion skids running through 2056.
How to use this manual
New to the lab: Overview, your Role card, your Zone card, the Cadence section. ~30 min.
Running an emergency: Section 7. Each procedure is one card with PPE, immediate steps, escalation.
Field service at year 10, 20, 30: Section 5. Each interval is its own procedure card with PPE, LOTO, BOM, sign-off.
Sourcing materials: Section 9 supply runbook.
Chemical safety: Section 6 Chemical Hygiene Plan + Section 7 emergency cards.
Print-friendly with section headers + page numbers per page. Controlled document — revision history maintained by PM; CHO co-signs safety-relevant changes. Companion experimental protocol at hub/03_protocol.html.
Phase 1 staffing · FTE roll-up
3.95 FTE across 6 named roles: PhD electrochemist 1.0 + Chemical Hygiene Officer 0.25 + instrument tech 1.0 (also CHO deputy) + lab tech 1.0 + program manager 0.5 + data engineer 0.2. Six headcount; 3.95 FTE budget. Hire all six by Stage 1 month 1; PhD electrochemist + instrument tech start in Stage 0 for facility commissioning.
Revision history
Rev
Date
Owner
Scope of change
CHO co-sign
1.0
2026-06-15
PM
Initial issue: 5 roles, 3 zones, 5 emergency procedures, 30-yr service single table, data + supply runbook.
n/a (CHO role not yet defined)
2.0
2026-06-15
PM
Added emergency procedure expansions; data table standards; supply runbook v1.
✓ CHO signed
3.0a
2026-06-16
PM
Lab-ops audit pass: throughput math reconciled (8/day×Mon-Fri = ~520 net of holidays + maintenance); 30-yr schedule exploded into 7 procedure cards; Zone equipment gaps closed (Karl Fischer, BET, XRD, TGA, DI polisher); supply runbook expanded; 20–25-yr cathode refurb card rewritten to work-instruction depth.
✓ CHO signed
3.0b
2026-06-16
CHO + PM
Chemical-hygiene audit pass: named CHO + Data Engineer roles; new §6 Chemical Hygiene Plan with HazCom + eyewash + NMP-specific + confined-space determination + EHS RACI; P030 ferrocyanide carve-out (complexed-cyanide, not P-listed); emergency procedures 5→12.
V5 final pass: standalone Respiratory Program (1910.134), BBP Exposure Control Plan (1910.1030), DOT 49 CFR 173.185 shipping spec, EAP (1910.38) + FPP (1910.39); 20-yr refurb FT-IR + half-cell method spec, SNT-TC-1A Level II NDE qualification, HCN reactor offgas scrubber spec; revision history table broken into per-pass rows; print-critical priority weight; CHP color folded into blue family.
✓ CHO signed
Section 2 · The Roles
The 6 Phase 1 Roles
Each role has defined Scope, Authority, and Reports-to chain. Decisions escalate along the chain; data flows through the program manager to Plantweb and to stakeholders.
Role 1
PhD Electrochemist (lead)
1.0 FTE
Scope
Decides chemistry variants, interprets cycler data, signals kill-gate triggers, prepares stage-gate reviews, named author on publications + patent disclosures.
Authority
Final call on chemistry variant priority, cell-build queue, kill-gate signal, data publication, contract-lab scope.
Owns + implements the Chemical Hygiene Plan per 29 CFR 1910.1450. SDS library, PPE Hazard Assessment, training matrix, waste-stream determinations, NaOCl detox, NMP / HNO3 / ferrocyanide hazards, Shakopee EHS liaison. Stop-work authority on any safety concern, no override.
Authority
Final call on PPE specification, waste-stream classification, training completion, emergency-response activation, stop-work.
Plantweb schema for Phase 1 telemetry, cycler-data ETL, dQ/dV pipeline reproducibility, cell-registry hygiene, LIMS/ELN (Benchling or eLabFTW), analysis-software version control. Frees electrochemist’s time from data plumbing.
Authority
Data schema, script versioning, ETL architecture, cell-registry naming, retention policies.
Reports to
PM. Coordinates with electrochemist + Emerson Plantweb team.
Daily
ETL pipeline health
dQ/dV automation on overnight data
Cell-registry sync with lab tech log
Weekly
Analysis-script commits + review
Plantweb schema redline
LIMS sync verification
Monthly
Pipeline reliability metrics
Data retention audit
Software version registry update
Section 3 · The Zones
The 3 Lab Zones
Flow-coupled: A purification feeds B assembly; B feeds C testing; recovery loop returns Cu and electrolyte back to A. Full floor plan in hub/04_floorplan.html.
Equipment: Rosemount 228 conductivity, Rosemount 372/RBI pH, Micro Motion ELITE Coriolis, ICP-OES with HNO3 digestion bench, electrowinning rig (emew/ElectraMet), rotovap solvent still, NaOCl in-line dosing with DeltaV control loop, Karl Fischer titrator (moisture is THE aqueous-Mg failure mode you cannot see with ICP), Type-II / Type-I DI water polisher (1–18 MΩ·cm), stir plates, vacuum filtration kit, lined carboys, 4-decimal balance, NIST-traceable standards (ICP, pH 4/7/10, conductivity).
PPE (29 CFR 1910.132): Face shield + acid-resistant gloves (butyl/neoprene, NOT nitrile) + lab coat + closed-toe for HNO3. Splash goggles + nitrile for routine electrolyte. Face shield + nitrile + apron for NaOCl. 5.8 M concentrated MgCl2 requires the same splash protection as any concentrated chloride solution (osmotic burn, slip, carbon-steel corrosion) — full splash protection required even though FDA food-grade.
Daily
Conductivity + pH baseline; ICP standards; NaOCl reservoir; Coriolis zero; Karl Fischer moisture on stock electrolyte.
Weekly
Fresh batch prep (4.0 M + sat 5.8 M); full ICP on retained samples; electrowinning bench rinse + electrode check.
Monthly
Full NIST-traceable calibration sweep; rotovap maintenance; NaOCl drill; Type-II water RO membrane health.
~40 cells Mon–Fri; materials prep; slurry-recipe verification; doctor blade alignment; gap gauge check.
Monthly
Materials inventory; glovebox catalyst regen (pyrophoric — see E-11); coating-thickness calibration; die sharpening; antechamber pump service.
Zone C
Testing
Cycling, characterization, environmental conditioning, postmortem. Where Phase 1 data lives. Cycler channels run 24/7.
Equipment: NI HPS-17000 multi-channel cycler (32+ channels), NI PXI EIS, environmental chamber (-40 to +85°C, humidity), BET surface area analyzer (electrode active mass), XRD diffractometer (PBA framework verification per §9 qualification), TGA (binder decomposition + moisture in electrodes), micrometer (electrode thickness post-calendar), Mettler 5-place balance (sub-mg active mass), water-activity meter, lab-grade DC load bank, electrical LOTO station. EQCM + Raman contract-lab routed in Phase 1 (NI Austin for Raman; EQCM deferred unless Stage 0 expert review demands).
PPE: Arc-flash rated PPE for any cycler bus work above 50 V DC (NFPA 70E; see E-10). Standard safety glasses + lab coat for routine. Cryo gloves + face shield for env chamber low-temp intervention.
Daily
Cycler channel-status; env chamber logs; EIS reference-cell baseline; data archive to Plantweb via ETL.
Weekly
Capacity-retention curves for top cells; dQ/dV batch; env chamber recal; cell shipping prep for Raman.
Throughput math: 8 builds/day × Mon–Fri = 40/wk × ~13 working months net of holidays + monthly maintenance windows ≈ ~520 total cells. Formation cycling adds 24–72 hr per cell on top of build time; channel allocation rule (see formation note below) governs how the 32 cycler channels keep the test pool full.
Formation cycling: newly assembled cells need 24–72 hr at C/10 formation before meaningful cycling data. The cycler queue maintains a formation pool ahead of the active-test pool; electrochemist allocates channels weekly. Channel demand exceeds 32 supply by week 6; rolling allocation rule established at week 4.
Weekly Rhythm
Day
Who
What
Monday 07:00–08:00
Instrument tech
Equipment maintenance window (moved from Wednesday to avoid build-day collision): cycler cal, EIS check, glovebox regen, consumables reorder.
Field-service schedule for deployed skids, intervals from annual through 30-year disposition. Each interval is its own procedure card with PPE, LOTO, BOM, acceptance criteria, sign-off lines.
Continuous
Plantweb Monitoring
Online; no downtime
Scope
Real-time telemetry: electrolyte conductivity (Rosemount 228), pH (Rosemount 372/RBI), Cu leach rate (inline ICP), cell capacity retention (NI cyclers), gas evolution (H₂/O₂), voltage hysteresis, temperature, vibration. Standard Plantweb dashboard.
24–48 hr · offline · electrolyte stays in sealed modules
Site-class note
Indoor / climate-controlled: may extend repaint to 15–20 yr if 5-yr inspection shows minimal coating progression. Outdoor coastal / chloride: holds to 10-yr cycle. CHO + field-service lead determine site class at first commissioning.
PPE
Wet abrasive blast: respirator (P100 silica-free; supplied air for silica), eye, hearing, full chem-resistant coveralls, gloves. Paint: organic-vapor cartridge respirator, chem-resistant gloves, coveralls.
LOTO
Full LOTO all systems. Arc-flash assessment per NFPA 70E before BMS enclosure access.
Surface-prep specs
Wet abrasive blast (preferred at chloride sites). Target: SSPC-SP10 / NACE No. 2, near-white metal, 2–3 mil profile. Holiday test per ASTM D5162. Ambient 50–90°F; surface ≥5°F above dew point; RH <85%. Recoat window per primer datasheet.
Coating system
Zinc-rich primer (Hempel Hempadur Zinc 17360 or eq.), 3–4 mil DFT. Epoxy intermediate (Hempadur Mastic 45880 or eq.), 4–6 mil DFT. Polyurethane topcoat (Hempathane 55610 or eq.), 2–3 mil DFT. Match fleet color standard. Total DFT 9–13 mil.
BMS hardware refresh to next-gen Zitara (hot-swappable).
Rosemount sensors recalibrated or upgraded.
Pump full refurb (bearings, impellers, seals).
Valve trim replacement (any flagged at 10-yr).
Cable insulation inspection on Cu interconnects (megger if flagged).
LOTO removal, recommission.
Acceptance
BMS recommissions to next-gen firmware; Plantweb telemetry confirmed; all Rosemount sensors pass post-cal verification (within manufacturer tolerance); pumps run within spec vibration (<0.15 in/s RMS per ISO 10816) + temperature (<10°F above ambient); valve trim leak-test pass at 1.5x operating pressure; Cu cable megger >100 MΩ @ 500 V DC.
1–2 weeks · offline · ~1–2% of fleet at any time · runs at Emerson refurb facility
Precondition
Procedure runs at the Emerson refurb facility (centralized, instrumented, supplied-air-equipped). Customer-site cathode refurb is not in scope. Process specs in this card pending Phase 3 pilot validation; chemistry precedent is standard hydrometallurgical practice for PBA-type cathode materials — specifically Hoffman 1996 for Cu electrowinning + Lee 2017 for aqueous PBA re-precipitation.
HCN hazard control
Ferrocyanide [Fe(CN)6]4− stable under standard conditions. HCN liberation threshold: sustained temperature ≥100°C OR pH ≤4.0 in presence of [Fe(CN)6]4−. Hazard control: entire re-dissolution operated at pH 5.5–6.5 (target 6.0 ± 0.3) and T ≤80°C (target 60°C); continuous HCN ambient monitoring (Drager Pac 8000 or equivalent) at ≤1 ppm alert / ≤4.7 ppm STEL. Any excursion triggers E-8 procedure + facility evacuation. Reactor offgas treatment: reactor headspace vented through a caustic scrubber column — packed-bed (1-inch Pall rings or equivalent), 10–15% w/w NaOH solution recirculated, residence time ≥3 sec, outlet HCN continuously monitored (Drager downstream) with breakthrough alarm at 0.5 ppm. NaOH scrubber liquid replaced when free OH- drops below 5% w/w; spent scrubber liquid contains soluble [Fe(CN)6]4− / cyanate — handled per CHP waste-stream (non-listed; characterized per MPCA guidance).
PPE
Full chem-resistant coveralls (Tychem 4000 or equivalent), face shield over splash goggles, supplied-air respirator (NOT cartridge) during stages 4–7 below, butyl gloves (8 mil min, double-glove for direct contact), chemical-resistant boots, closed-toe steel-toe. Cyanokit (hydroxocobalamin 5g IV) on standby in refurb facility medical bay; designated first-responder on shift.
LOTO + permits
Full LOTO on skid systems before disassembly per 29 CFR 1910.147. Permit-to-work (hot work) if any welding required for collector replacement. Confined-space permit per 1910.146 if skid interior access required (typically not — cells removable from external access).
Electrolyte handling: lined transport tankers (HDPE or polypropylene, food-grade), peristaltic transfer pumps (chloride-rated), DI water polisher output for refresh (Type II, >1 MΩ·cm).
PBA re-precipitation: 200-L jacketed glass-lined reactor (T-controlled to ≤80°C), pH meter (Rosemount 372 or eq.), continuous HCN monitor (Drager Pac 8000 or eq., 0–10 ppm range, audible alarm @ 1 ppm), magnetic stirrer (variable-speed).
Cu electrowinning: emew rotating-cathode rig (preferred) OR ElectraMet plate rig. Operating: current density 200–400 A/m2; cathode area 0.5–2.0 m2; cell voltage 2.0–2.5 V; bath temperature 40–55°C; H2SO4 bath conductivity >30 S/m. Cu plate harvested at 5–10 mm thickness.
Reagents (refresh): battery-grade MgCl2·6H2O (Nedmag or qualified second source); CaCl2·2H2O (commodity); Type-II DI water (on-site or Avantor totes); reagent-grade Na2CO3 for pH buffering during re-precipitation (not added to final electrolyte).
Replacement parts: GF/A separator sheets (Whatman or qualified second source; cut to module-specific geometry); SS 316L collector foil (25 µm, 0.5×0.5 m sheets); upgrade-spec collectors: 904L or duplex 2205 (if 5-yr inspection fleet pattern indicates pitting); fresh COP anode active mass (synthesized at refurb facility or contract-sourced — lot tied to refurb skid serial).
Drawings: skid as-built drawing series SWP-SKD-XXXX (per skid serial); cell module drawing SWP-CM-XXX; collector geometry SWP-CC-XXX. All on file at refurb facility.
Procedure (refurb facility, ~1–2 wk)
Receive skid from customer site (electrolyte drained for transit per BaaS protocol; transport-tanker accompanies skid). Verify Plantweb baseline matches dispatch baseline.
Apply LOTO on all skid systems. Verify de-energized per E-10.
Refill skid with transport-tanker electrolyte for in-skid Cu recovery cycle (operate at 0.5C for 24 hr to drive residual Cu to electrowinning loop). Acceptance: in-skid ICP shows Cu <30 ppm before module removal.
Drain electrolyte into refurb-facility holding tanks for full processing. Verify HCN monitor <0.5 ppm throughout drain.
Remove cell modules from skid frame via jib crane to module transport cradle. Tag each module with skid serial + module position + removal-date for re-stack tracking.
Dissolve recovered PBA mass in 0.5 M Na2SO4 at T = 60°C, pH 6.0 ± 0.3, stirring 200 rpm, 4–6 hr until full dissolution.
Verify HCN ambient <1 ppm at each 30-min interval; halt + evacuate if ≥1 ppm.
Cool solution to 40°C; re-precipitate CuFe-PBA via controlled addition of FeSO4·7H2O (3% excess Fe stoichiometry) over 60 min; maintain pH 6.0 ± 0.3 with Na2CO3 drip.
Age precipitate 12 hr at 25°C; filter, rinse 3× with Type-II DI water; vacuum dry 24 hr at 60°C.
QA: XRD pattern match against reference CuFe-PBA (Whateley 2024 reference); ICP Cu/Fe ratio within 0.95–1.05; BET surface area within ±15% of original lot; particle size distribution D50 within ±20% of original.
Cu electrowinning: mother liquor + dissolved Cu fraction to electrowinning rig. Operating per BOM spec. Harvest Cu plate at 5–10 mm thickness; weigh; mass-balance vs original Cu inventory. Target: ≥95% Cu recovery by mass.
COP anode reconditioning: assess by FT-IR + electrochemical half-cell test.
FT-IR: ATR mode, scan range 400–4000 cm-1, resolution 4 cm-1, 32 scans averaged. Compare to reference Hex-TADD-COP spectrum (radical-cation marker at 1620 cm-1; degradation indicator: hydroxyl/carbonyl growth at 3200–3500 / 1700 cm-1).
Electrochemical half-cell: 3-electrode Swagelok, COP working / Pt counter / Ag/AgCl reference, 4.0 M MgCl2 aqueous electrolyte, scan range -1.0 to +1.0 V vs Ag/AgCl, 5 mV/s CV; 20 cycles formation then 100 cycles at C/4. Capacity ratio vs original commissioning baseline.
Decision: capacity >85% of original → recondition by N2-flow thermal cycling at 80°C / 12 hr; capacity <85% → replace with fresh COP from refurb-facility synthesis.
SS 316L collector inspection: visual + microscopic; replace any with pit depth >25% of foil thickness per ASTM G46. Upgrade trigger: if >30% of fleet collectors at this refurb event show pitting >15% thickness, upgrade to 904L or duplex 2205 for the refurb cohort (CHP redline + skid as-built update).
Frame inspection: ultrasonic weld inspection (ASME Sec V Art 4) on all primary structural welds — NDE qualification: technician minimum SNT-TC-1A Level II with documented PQR on this material class (carbon steel for primary frame; SS 316L for chloride-contact welds). Visual + dye-penetrant on secondary welds per ASME Sec V Art 6. HDPE tank fitting inspection (visible stress cracking, fitting torque per as-built); pressure-test tanks at 1.5× operating pressure for 30 min.
Electrolyte refresh: blend processed transport-tanker electrolyte (~70% recovered) with fresh battery-grade MgCl2 + CaCl2 + Type-II DI water to reach original-spec concentration (4.0 M MgCl2 + 1.0 M CaCl2, pH 7.0 ± 0.3). ICP-OES verify Mg/Ca ratios + trace metals against Nedmag spec.
Re-stack cells with refurbed cathode mass + fresh separator + inspected/upgraded collectors. Torque per as-built (typically 35–50 in-lb on cell hardware; verify against SWP-CM-XXX). Cell-level commissioning per §protocol 03_protocol: 5 formation cycles at C/10, verify capacity, EIS spectrum match.
Re-insert modules into skid frame; torque module hold-down per as-built (typically 80–120 ft-lb); reconnect electrical bus per as-built; verify Cu interconnect torque per E-10 spec.
Refill skid with refreshed electrolyte; pressure-test all wet-side fittings.
Remove LOTO; re-energize; recommission to new Plantweb baseline. 7-day burn-in at 0.5C with continuous Plantweb monitoring before customer delivery.
Ship back to customer site (drained for transit; refilled on arrival per BaaS protocol).
Acceptance criteria
Cu recovery: ≥95% of original Cu mass.
PBA re-precipitate: XRD match Q>0.92 vs reference; Cu/Fe ratio 0.95–1.05; BET within ±15%.
Cell capacity: 7-day burn-in average within 5% of original commissioning baseline.
HCN ambient: never detected >1 ppm during any procedure stage; CHO sign-off attests.
Structural inspection: all welds ASME Sec V Art 4 pass; HDPE tanks pressure-test pass at 1.5× operating.
Plantweb baseline: all telemetry signatures within 2σ of dispatch baseline post-burn-in.
Mass balance: total Mg + Ca + Cu + Fe recovered + replaced reconciles to within 1% of original inventory; any unaccounted mass triggers root-cause before customer dispatch.
Refurb facility lead: _________________ · Date: _________
CHO sign-off (HCN-free, all stages): _________________ · Cu recovery yield: ______ %
Cell capacity post-burn-in: ______ % of original baseline · Cell cycle CE: ______ %
Structural inspection (welds + tanks): □ Pass ·
Plantweb baseline post-recommission: □ Within 2σ · Mass-balance reconciliation: ______ % accounted
Customer dispatch authorized: _________________ · Date: _________
25–30-year
Decision Point
Strategic decision; not single procedure
Three paths
(a) Continue another decade: second cathode refurb cycle. Most common for hyperscaler / utility customers.
(b) Cells repurposed to second-life: UPS, telecom backup, behind-the-meter peak shaving. Cells <80% capacity but stable Cu leach qualify.
(c) Full material recovery: MgCl2 to industrial salt supply; PBA recovered (~95% Cu via electrowinning); Ti foil + SS 316L to metals recycle; frame to scrap; BMS to Emerson refurb pool.
Decision authority
Customer + Emerson asset team jointly. Default to (a) unless economics + sustainability favor (b) or (c). BaaS-fleet skids may bypass customer choice if Emerson redeploys.
Section 6 · Chemical Hygiene
Chemical Hygiene Plan
Written program per 29 CFR 1910.1450 covering SDS library, HazCom, PPE Hazard Assessment, waste-stream determinations, training matrix, Shakopee EHS interface. Maintained by named CHO; co-signed by PM; reviewed monthly with Shakopee EHS.
This plan implements the Laboratory Standard. The Chemical Hygiene Officer (Role 2) is named in writing and trained. CHP reviewed annually + re-certified by Emerson Corporate EHS. Material change requires CHO sign-off + redline log entry.
PPE Hazard Assessment matrix (29 CFR 1910.132)
Per-task assessment; signed annually by CHO + each lab member
Zone A · HNO3 digestion: face shield + acid-resistant gloves (butyl/neoprene, NOT nitrile) + lab coat + closed-toe + emergency shower within 10 sec reach.
Zone A · routine electrolyte: splash goggles + nitrile + lab coat. For 5.8 M concentrated — full splash + face shield.
Zone A · NaOCl: face shield + nitrile + apron + fume-hood-only.
Zone B · NMP slurry: nitrile (double for >5 min) + splash goggles + fume hood + lab coat.
Zone B · glovebox: butyl gauntlets (built-in); O2 monitor operational before any work.
Zone C · cycler bus >50 V DC: arc-flash rated PPE per NFPA 70E + LOTO active.
Zone C · env chamber low-temp: cryo gloves + face shield for <0°C intervention.
Waste-stream determinations
EPA RCRA per 40 CFR 261 · satellite accumulation per 40 CFR 262.15 · POTW permit required for sewer discharge
Spent MgCl2/CaCl2 (uncontaminated): FDA food-grade; sewer-eligible after dilution + Shakopee POTW pretreatment permit. Permit obtained pre-opening; copy in CHP appendix.
Ferrocyanide solutions: K4[Fe(CN)6] is a complexed-cyanide, NOT P-listed (P030 covers soluble cyanides only: NaCN, KCN). Classify as non-listed; characterized per MPCA guidance; treat as D003 reactive if heat or acid exposure is foreseeable. Storage labeled, no acid contact, kept below 100°C. CHO confirms case-by-case characterization with MPCA at lab opening.
Emergency response: Shakopee Fire Response primary first responder; campus 911 escalation; CHO + PM notified within 5 min via Plantweb alert + redundant SMS.
Mutual aid: MN State HAZMAT Region 6 auto-activates for large chemical spill or mass casualty exceeding Shakopee EHS capability.
Standalone Respiratory Protection Program (29 CFR 1910.134)
Required where any worker wears a respirator — NMP cartridge, supplied-air for HCN/Cl2/O2-deficient, P100 for blast operations
Program administrator: CHO maintains the written program; deputy is the instrument tech.
Medical clearance: PLHCP-administered OSHA Respirator Medical Evaluation Questionnaire (Appendix C) before any respirator use; written authorization required before fit-test. Recurrence: annually for supplied-air users; on change-of-status for cartridge users.
Fit-testing (1910.134(f)): qualitative (saccharin/Bitrex) acceptable for half-face cartridge; quantitative (PortaCount) required for full-face and supplied-air. Annual + on facial-hair / weight change / dental change.
Cartridge change schedule (1910.134(d)(3)(iii)): NMP organic-vapor cartridges — pre-end-of-service-life indicator OR scheduled change at lesser of (8 hr cumulative service / odor threshold detected / manufacturer’s service-life recommendation). Cartridge inventory + change log in Plantweb respiratory module.
Supplied-air specification: Grade D breathing air per CGA G-7.1 (oxygen 19.5–23.5%, condensed hydrocarbons ≤5 mg/m3, CO ≤10 ppm, CO2 ≤1000 ppm, lack of noticeable odor). Compressor air-line testing quarterly; CO monitor on compressor outlet with high-CO shutdown. Cascade cylinder backup for HCN-procedure stages 4–7 of the 20-yr refurb.
Voluntary use: any worker who voluntarily wears a dust mask must receive Appendix D information (no fit-test required).
Maintenance: half-mask + full-face cleaning daily after use, monthly disinfection per manufacturer; storage in sealed bag in clean area.
Records: medical evaluations 30 yr per 1910.1020; fit-test records until next test + 1 yr; written program reviewed annually.
Bloodborne Pathogen Exposure Control Plan (29 CFR 1910.1030)
Required where employees are designated to render first aid as a collateral duty — all 6 Phase 1 employees per training matrix
Exposure determination: all 6 employees designated as collateral-duty first responders for any zone incident; CHO + safety-officer rotation + the lab tech are the most likely responders given build-bench location.
Hepatitis B vaccination: offered at no cost to each designated employee within 10 days of assignment. Declination requires signed Appendix A waiver. Vaccinations + declinations tracked in Plantweb employee-medical module (30-yr retention per 1910.1020).
Universal precautions: treat all human blood + body fluids as potentially infectious. BBP gloves + face shield required for first-aid response.
Sharps handling: the lab handles no needles routinely (no biological sampling); broken-glassware incidents managed with mechanical pickup tools (forceps, dustpan), never bare hands. Sharps container at lab entrance.
Engineering + work-practice controls: handwashing stations at every zone exit; eyewash + emergency shower per ANSI Z358.1; BBP cleanup kit (gloves + face shield + absorbent + disinfectant + biohazard bag) at lab entrance.
PPE for BBP response: nitrile gloves (minimum 2 pairs for any direct contact); face shield + safety glasses; isolation gown for splash potential.
Post-exposure procedure: immediate decontamination + medical evaluation by PLHCP within 2 hr. Source-individual testing per CDC guidance (with consent). Post-exposure prophylaxis per CDC if HIV/HBV/HCV risk identified.
Training: initial + annually thereafter; documented in employee training matrix.
Records: medical 30 yr; training 3 yr; sharps injury log if any.
DOT shipping spec for cells + samples (49 CFR 173.185 et al.)
Cell shipments to contract labs (Raman/EQCM) and end-of-life cells to recycler require proper DOT classification
Aqueous Mg-ion cells — novel-chemistry classification: not covered under 173.185 lithium-battery provisions. Initial shipments classified as UN3496 Batteries, nickel-metal hydride by analogy (aqueous non-flammable rechargeable) OR pursued via DOT Special Permit (SP) application if 3496 classification is contested. Trade counsel + DOT consultant scope at Phase 1 first contract-lab shipment.
Packaging: tested non-spillable cells per UN 2.9.4; outer packaging meets PG II performance specifications; non-spillable orientation maintained with cushioning; metallic protection on cell terminals.
Labels + markings: proper shipping name, UN number, hazard class label (if applicable), shipper + consignee addresses, emergency response phone number (CHEMTREC contract or equivalent). “LITHIUM BATTERY MARKING” does NOT apply — do not use.
Hazard Communication Sheet (HCS) / Shipper Declaration: required for any DOT-classified shipment.
Spent-cell shipments to recycler: classified as universal waste battery per 40 CFR 273. DOT for universal waste batteries: 49 CFR 173.185(a)(7) provides exception if cells meet non-spillable + protected terminals; documented in CHP waste-stream protocol.
Hazmat employee training: CHO + PM complete 49 CFR 172.704 hazmat training (general awareness + function-specific + safety + security) at lab opening + every 3 yr; records retained 3 yr.
Emergency Action Plan + Fire Prevention Plan (29 CFR 1910.38 + 1910.39)
Standalone documents required for any workplace with employees
EAP (1910.38) — written plan covers: (a) alarm system + how it is activated; (b) evacuation routes + floor-plan diagram (full floor plan in hub/04_floorplan.html); (c) procedures for employees who remain to operate critical operations before evacuation (instrument tech secures glovebox + cycler queue); (d) accountability procedures after evacuation (PM or CHO performs head-count at Shakopee muster point); (e) procedures for reporting fires + emergencies; (f) names + job titles of designated employees + duties; (g) training (initial + when plan changes + when employee role changes).
Alarm system: Shakopee campus alarm with pull stations at lab entrance + at each zone exit. Audible + visual signals throughout. Tested monthly per Shakopee EHS schedule.
Evacuation routes: primary route through lab entrance to main corridor + south stairwell to ground floor + south parking lot muster point; secondary route through Zone C emergency exit. Routes posted at every zone exit.
FPP (1910.39) — written plan covers: (a) list of fire hazards: NMP (flashpoint 91°C, Zone B fume hood), organic precursors (solvent still Zone A), electrical equipment in all zones, glovebox catalyst pyrophoric byproducts (E-11); (b) procedures to control accumulations of flammable materials (regular waste removal; NMP storage in flammable cabinet meeting NFPA 30); (c) procedures for maintenance + safeguarding heat-producing equipment (annual inspection + cleaning); (d) names of personnel responsible for control of fuel-source hazards (CHO + instrument tech); (e) housekeeping standards (combustibles <1 day’s accumulation).
NFPA 30 storage: NMP + organic precursor inventory tracked + stored in approved flammable-liquid cabinet, max 60 gal per cabinet; total lab inventory <120 gal of flammables per NFPA 30 Table 9.6.
Training: EAP + FPP training at lab opening + when plan changes + employee assignment changes.
Standalone Hazard Communication program (29 CFR 1910.1200)
Required separate from CHP; produced on inspector request
Chemical inventory: master list maintained by CHO in Plantweb chemical-inventory module; every container in the lab is on it within 24 hr of receipt.
Container labeling: GHS-compliant labels (pictograms + signal word + hazard statements + precautionary statements) on every secondary container at point of fill. Original manufacturer labels retained on primary containers.
SDS access: all SDS available through (a) lab Plantweb SDS portal accessible from any workstation, (b) printed binder at lab entrance for power-outage redundancy, (c) Shakopee EHS master SDS library backup.
Employee training records: initial HazCom training at hire + retraining whenever new hazard introduced. Records in employee file + Plantweb training-matrix module.
Non-routine task hazard assessment: any first-time use of a chemical requires CHO walkthrough + signed SDS-review before work begins.
Multi-employer worksite communication: contractors (painters, electricians, vendor service) get HazCom briefing on lab chemistry before entry.
Eyewash + emergency shower (ANSI Z358.1)
Weekly activation + annual full-flow test, documented; 10-second/no-obstruction travel-distance for HNO3 areas
Locations: Zone A (within 10 sec / 55 ft of HNO3 digestion bench + NaOCl station); Zone B (near fume hood); Zone C (general); all locations unobstructed, well-lit, marked with high-vis signage.
Weekly activation test: CHO or designee activates each eyewash for ~3 seconds; verifies flow + temperature + signage. Logged in Plantweb safety module.
Annual full-flow test: third-party or trained internal tests per ANSI Z358.1 (15-min minimum flow at 0.4 gpm; 60–100°F tepid water; ANSI-compliant pattern). Calibration certificates retained.
Out-of-service procedure: any non-operational station triggers immediate work-restriction in that zone until repaired or temporary replacement installed.
Travel distance: from any HNO3 work position, eyewash reachable within 10 seconds unobstructed. Verified during PPE Hazard Assessment annual review.
NMP-specific exposure control (TSCA §6 Dec 2024 rule)
NMP reproductive toxin Cat 1B GHS; dermal-route is dominant exposure path; PEL 1 ppm TWA / 5 ppm STEL
Glove specification: 8-mil nitrile minimum for incidental contact; double-glove for any contact >5 min. Butyl, laminate (Silver Shield), or 4H gloves required for any pour, transfer, or extended-contact work — NMP penetrates standard nitrile in <30 min.
Glove change cadence: change every 2 hours regardless of visible contamination; immediately on visible wet contact.
Engineering controls: fume hood required for any open container; sash position verified daily by CHO.
Respiratory protection: if measured exposure approaches PEL, fit-tested half-face respirator with organic-vapor cartridge per 1910.134 + medical clearance.
Pregnant-worker accommodation: any worker who may be pregnant must consult Emerson Occupational Health before NMP work; alternative task assignment available without prejudice; CHO maintains the request channel discreetly.
Substitution evaluation: Phase 1.5 evaluates CMC/SBR aqueous binder as NMP alternative — if technical performance acceptable, transition all slurry work to aqueous binder per CHP redline.
Exposure monitoring: personal air-monitoring quarterly for the lab tech (primary NMP user); records retained 30 yr per 1910.1020.
Confined-space determination (29 CFR 1910.146)
Phase 1 written determination — revisit at Phase 2 if cell modules or skid interiors enter scope
Determination for Phase 1 coin-cell lab:No permit-required confined-space (PRCS) entries are anticipated. All work occurs in open lab space with adequate ventilation. Glovebox antechamber, environmental chamber, and electrowinning bench are NOT PRCS by 1910.146 definition (limited entry/exit + unfavorable atmosphere + not designed for continuous occupancy — none meet all three criteria at Phase 1 scale).
Trigger conditions for future PRCS program: if any of the following emerges at Phase 1.5 / 2 / 3, a written 1910.146 PRCS program must be in place before that activity begins: (a) entry into sealed cell modules at pouch or skid scale; (b) interior inspection of electrolyte reservoir tanks; (c) entry into refurb-facility skid interiors during cathode refurbishment.
Phase 1 inert-gas hazard control (E-9 inert-gas asphyxiation) is managed via ambient O2 monitor + ventilation, not via PRCS program, because the inert-gas release scenario in open lab space is rescue-managed by supplied-air respirator rather than confined-space entry permit.
Section 7 · Emergency
Emergency Procedures
All twelve procedures, each as an independent card. If you’re reading this in an emergency, scan the red header bars for the matching E-number. Each card carries PPE, immediate steps, escalation, and follow-up paperwork. Stop-work authority rests with the CHO and any employee; no override.
E-1Priority: low
Electrolyte spill (Zone A or B)
PPE
Splash goggles + nitrile + lab coat + closed-toe minimum. Add face shield + butyl if 5.8 M concentrated. SDS index in Zone A binder + Plantweb.
Steps
Stop the source. Close valves; verify with Plantweb leak-detection alert.
Contain. Spill berm or absorbent socks. Zone A drawer A-3.
Assess volume. <1 L routine; 1–10 L notify CHO + PM; >10 L stop-work + notify Shakopee EHS within 30 min.
Cleanup. <1 M FDA food-grade no neutralization. 5.8 M concentrated requires full splash PPE through cleanup (osmotic burn risk, slip hazard, carbon-steel corrosion). Absorbent pickup per CHP waste-stream. Rinse with DI; conductivity check.
Document. Lab notebook + Plantweb event log; CHO reviews.
Escalation
CHO within 15 min; PM within 1 hr; Shakopee EHS if >10 L or repeated.
Follow-up
Root-cause memo within 48 hr; procedure update if needed.
E-2Priority: medium
Glovebox atmosphere failure
PPE
No additional beyond standard zone PPE. If gas release suspected, evacuate + see E-9.
CHO + PM immediately; Shakopee EHS within 30 min; Logan + Muck within 2 hr regardless of severity.
Follow-up
OSHA-compliant incident report within 24 hr; root-cause within 7 days.
E-6Priority: critical
HNO3 acid burn / exposure
Context
Concentrated HNO3 (15.8 M, ~70%) used in ICP-OES digestion. OSHA PEL: 2 ppm TWA / 4 ppm STEL (inhalation). Skin: corrosive Cat 1 GHS — direct contact = severe chemical burn within seconds.
PPE (should have)
Acid-resistant gloves (butyl/neoprene — not nitrile) + face shield + lab coat per Zone A PPE matrix.
Steps
Stop-work for zone.
Eye exposure: immediate 15-min eyewash; call 911 + Shakopee EHS during flush; do not delay flush to call.
Skin: emergency shower ≥15 min; remove contaminated clothing during shower.
Inhalation: fresh air; call 911; delayed pulmonary edema possible — medical eval required even if asymptomatic.
Ingestion (rare): do NOT induce vomiting; call 911 + poison control.
Spill cleanup: after personnel safe, neutralize with sodium bicarbonate; CHP waste-stream protocol.
Escalation
911 + CHO + PM simultaneously; Shakopee EHS within 30 min; Logan + Muck within 2 hr.
Follow-up
OSHA recordable; PPE assessment review; medical surveillance for inhalation.
E-7Priority: high
NMP solvent exposure / inhalation
PPE (should have)
Nitrile (double if >5 min) + splash goggles + fume hood per Zone B PPE matrix. NMP PEL: 1 ppm TWA, 5 ppm STEL.
Steps
Fresh air immediately. NMP reproductive toxin (Cat 1B GHS).
Skin: remove contaminated clothing; wash 15 min with soap + water.
Eye: 15-min eyewash; medical eval.
Inhalation (above PEL): medical eval required; HAZWOPER surveillance if significant.
Pregnancy concerns: NMP reproductive toxin — pregnant worker exposed must consult occupational health immediately.
Ferrocyanide salts (K4[Fe(CN)6] in PBA synthesis) stable at room temp + non-toxic standard conditions. Above ~100°C or in strong acid can liberate HCN. Triggers: heated decomposition, acid contact during electrowinning, fire.
PPE
HCN suspected: supplied-air respirator (NOT cartridge); evacuate; Cyanokit in Shakopee medical bay.
Steps
Evacuate immediately. HCN acutely toxic (death within minutes at high concentration).
Call 911 + state “possible cyanide exposure”; CHO calls Shakopee EHS simultaneously.
Symptoms: headache, dizziness, rapid breathing, almond breath odor, loss of consciousness. If unconscious/severe: Cyanokit (hydroxocobalamin) by EMS — do not delay transport.
Source control: only after personnel evacuated + triaged. Shakopee Fire / MN HAZMAT handles source. Do NOT re-enter without supplied-air + atmospheric clearance.
Post-incident: ventilate; air-monitor for HCN before re-entry; full root-cause.
Escalation
911 + Shakopee EHS + Fire immediately; PM + Logan + Muck within 1 hr; MN HAZMAT Region 6 auto-activates.
Follow-up
OSHA recordable; full process review; ferrocyanide handling SOP redline; storage review.
E-9Priority: high
Inert-gas asphyxiation (Ar / N2 release)
Context
Glovebox or Ar/N2 leak in enclosed space drops O2 below 19.5% (OSHA confined-space threshold) within minutes. No warning — victim loses consciousness without sensation of suffocation.
PPE
Rescue: supplied-air respirator. Cartridge respirators DO NOT protect against O2 deficiency.
Steps
O2 monitor alarm: evacuate immediately. Do not re-enter without supplied-air.
Call 911 + Shakopee EHS.
Victim down inside zone:do NOT enter without supplied-air respirator. Wait for trained rescue. Standard cartridges do not protect. Many rescuer deaths in O2-deficient incidents.
Victim removed to safe atmosphere: O2 if available; CPR if no pulse; AED.
Source control: shut off Ar/N2 at zone main; ventilate; air-monitor before re-entry.
Escalation
911 + Shakopee EHS + Fire immediately; PM + Logan + Muck within 1 hr.
NI HPS-17000 channels at full string voltage hazardous. Cu electrowinning DC bus likewise. Arc-flash assessment per NFPA 70E required before work above 50 V DC.
PPE
Arc-flash rated per NFPA 70E + skid label: arc-rated face shield, coverall (Cat 2 min, up to Cat 4), arc gloves with leather protectors, dielectric boots.
Steps
Arc-flash event: call 911 + CHO + Shakopee EHS; do not approach until power confirmed off.
Victim: assume serious burns + cardiac arrhythmia; do not move unless immediate danger; await EMS.
Power isolation: qualified electrician only; verify with calibrated voltage tester.
PROACTIVE LOTO before electrical work: (a) shutdown notice; (b) shutdown procedure; (c) isolate energy; (d) apply locks + tags; (e) release stored energy (capacitor discharge); (f) verify de-energization with calibrated tester; (g) begin work; (h) reverse to restore.
After incident: full electrical-safety review; equipment inspection; do not re-energize until cleared.
Escalation
911 + Shakopee EHS + Fire immediately; PM + Logan + Muck within 1 hr; Emerson Corporate EHS within 4 hr.
Follow-up
OSHA recordable; arc-flash assessment refresh; LOTO program audit; possible NFPA 70E training refresh.
E-11Priority: high
Pyrophoric event (glovebox catalyst regen)
Context
MBraun Cu-based regen catalyst can become pyrophoric if water-saturated then exposed to air. This card covers event response if regen procedure safety steps fail.
PPE
Fire-rated gloves + face shield + Class D extinguisher (combustible metals); Class B standard for solvent ignition.
Steps
Smoking / ignition during regen: stop airflow to catalyst; isolate from oxygen.
Do NOT use water on metal catalyst fires.
Fire propagates: Class D extinguisher (dry powder for combustible metals).
Evacuate if smoke significant; treat as E-3.
Vendor escalation: MBraun field service for regen procedure review.
Escalation
CHO immediately; Shakopee Fire if uncontained; PM; vendor coordination.
Follow-up
Regen SOP redline; MBraun coordination for catalyst handling refresh.
E-12Priority: high
NaOCl + organic incompatibility (Cl2 evolution)
Context
NaOCl (detox reagent Zone A) reacts with organic solvents to liberate chlorine gas. Particularly dangerous with NMP, amines, or acidic organic.
PPE
Cl2 released: supplied-air respirator; evacuate. Cartridge with acid-gas as backup.
Source control: ventilation; do NOT attempt source intervention without supplied-air.
Escalation
911 + Shakopee EHS + Fire immediately; PM + Logan + Muck within 1 hr.
Follow-up
NaOCl handling SOP redline; Zone A chemical-segregation audit; CHP storage-compatibility review.
Section 8 · Data
Data Recording Standards
What gets logged, where it goes, what triggers escalation, what gets retained, what supports patent prosecution. Plantweb is the SSO for telemetry + operational records; the LIMS / ELN (Benchling / eLabFTW) is the SSO for chemistry recipes + slurry batches + electrode lot genealogy. The paper lab notebook supports inventorship + trade-secret defensibility — under post-AIA first-inventor-to-file (March 2013), patent priority is established by filing date, not notebook date.
Scanned weekly to Plantweb; original in fire-rated cabinet
Per-entry
Permanent (IP)
IP-relevant entries: witness signature same-day; scan + index within 7 days. Supports inventorship; patent priority is filing date.
Cell library / postmortems
Lab tech inventory
Plantweb cell-registry; Zone C cold storage 24 mo
Per-build
30 yr metadata; 24 mo physical (matches §5 fleet aging dataset reach-back)
Unexpected failure mode → postmortem within 48 hr
Materials inventory
Lab tech monthly
Plantweb inventory module
Monthly + rolling 7-day reorder
7 yr
Consumable <30-day projected: PM notified
Calibration certificates
All instruments (NIST-traceable)
Plantweb calibration registry
Per-calibration
30 yr
Out-of-tolerance: back-flag affected data; data eng + electrochemist review
Equipment maintenance log
Instrument tech
Plantweb equipment-history
Per-event + monthly summary
30 yr
Unplanned downtime >4 hr; repair quote >$5K
Analysis software version
Data eng
Plantweb + git repo
Per-commit
30 yr
Any script change affecting published or stage-gate data
Sample chain-of-custody
PM + lab tech
LIMS chain-of-custody
Per-shipment to contract lab
30 yr
Any custody break or sample loss
Stage-gate review packet
Electrochemist + PM
Plantweb stage-gate folder
Monthly + on-trigger
Permanent
Stage 0 written go/no-go; Stage 1 quarterly; any kill-gate
Safety incidents + near-misses
CHO
Plantweb incident log + Shakopee EHS report
Per-event + monthly summary
30 yr
Any incident: same-day PM; within 30 min Shakopee EHS
Budget burn
PM + Emerson finance
Plantweb dashboard + weekly report
Weekly
7 yr
Burn >10% over projection in rolling 30-day window
Patent posture (post-AIA, March 2013)
US patent priority is established by filing date under first-inventor-to-file. Witnessed paper notebooks support inventorship determination in dispute and trade-secret defensibility — they do not establish patent priority. The LIMS/ELN + Plantweb form the operational record; the paper notebook is the inventorship + trade-secret backstop. Both retained permanently for IP-relevant entries.
Section 9 · Supply
Supply Chain Runbook
Qualified suppliers for every Phase 1 consumable + capital equipment. Dual-source resilience: at least two qualified vendors per critical material. Whatman GF/A second-source qualification pulled into Phase 1 (8–12 wk qualification cycle starts immediately, not deferred to Phase 3).
Qualification (tightened): ICP-OES verification on each lot vs COA. Absolute caps on trace metals (not relative drift): Fe <5 ppm, Cu <2 ppm, Ni <2 ppm, Mn <5 ppm. Cl- surface-contamination check. Reject failing lots.