--- lang: en-CA documentclass: article papersize: letter fontsize: 9.5pt geometry: margin=0.68in,headheight=18pt,headsep=16pt,footskip=25pt mainfont: "DejaVu Serif" sansfont: "DejaVu Sans" monofont: "DejaVu Sans Mono" colorlinks: true linkcolor: NanoNavy urlcolor: NanoBlue toc: false header-includes: - | \usepackage{xcolor,colortbl,fancyhdr,titlesec,booktabs,longtable,array,enumitem,microtype} \definecolor{NanoNavy}{HTML}{24364B} \definecolor{NanoBlue}{HTML}{496B86} \definecolor{NanoPale}{HTML}{E8EEF3} \definecolor{NanoRule}{HTML}{9AAABA} \pagestyle{fancy}\fancyhf{} \fancyhead[L]{\small\sffamily\color{NanoNavy} NANOARC $\mid$ Cell Qualification} \fancyhead[R]{\small\sffamily\color{NanoBlue} Rev0} \fancyfoot[C]{\small\color{NanoNavy}\thepage} \renewcommand{\headrulewidth}{0.4pt} \titleformat{\section}{\Large\bfseries\sffamily\color{NanoNavy}}{\thesection.}{0.55em}{} \titleformat{\subsection}{\large\bfseries\sffamily\color{NanoBlue}}{\thesubsection}{0.55em}{} \renewcommand{\arraystretch}{1.22} \setlength{\parindent}{0pt}\setlength{\parskip}{4pt} \setlist{nosep,leftmargin=1.45em} \hypersetup{pdftitle={NanoArc PCM Test Cell Qualification Rev0},pdfauthor={NanoArc thermal development},pdfsubject={Blank and standard cell qualification workbook}} --- \begin{titlepage} \thispagestyle{fancy} \vspace*{0.75in} \begin{center} {\Huge\bfseries\sffamily\color{NanoNavy} NanoArc PCM Test-Cell\\Qualification Workbook}\par \vspace{0.25in} {\Large\color{NanoBlue} Incoming Inspection, Water Blanks, and Thermal Baseline}\par \end{center} \vspace{0.45in} \rowcolors{1}{NanoPale}{white} \begin{tabular}{>{\bfseries}p{1.15in}p{4.55in}} Status & Approved protocol; no qualification run completed \\ Revision & Rev0 \\ Date & 2026-08-13 \\ Design & NanoArc 5 g PCM Test-Cell Family Rev0 \\ Authority & Tristan approves fixture release and cell qualification \\ \end{tabular} \rowcolors{1}{}{} \par \vspace{0.42in} This workbook qualifies practical laboratory use of the cell fixture. It does not establish a pressure rating, production cartridge, or Rumi safety/duty-cycle claim. \vfill \fcolorbox{NanoRule}{NanoPale}{\parbox{0.91\textwidth}{\textbf{Stop rule.} Stop immediately on glass damage, leakage, stopper movement, sensor disagreement, uncontrolled heating, bath boil-dry, guard failure, or any unexpected pressure indication.}} \end{titlepage} \tableofcontents \clearpage # Campaign identification | Field | Record | |---|---| | Campaign ID | | | Operator | | | Date range | | | Vial supplier / part / lot | | | Stopper supplier / part / lot | | | PTFE tape supplier / lot | | | Kapton tape supplier / lot | | | Fixture revision / photo directory | | | Webcam file directory | | | Tristan authorization | | # Incoming inspection Inspect every pilot vial under strong light. Reject chips, scratches, cracks, bubbles affecting the wall, neck damage, contamination, or closure defects. Never engrave the glass. | Cell envelope ID | OD mm | Height mm | Empty mass g | Neck/closure fit | Visual result | Disposition | |---|---:|---:|---:|---|---|---| | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | | | | | | Pass / Fail | Pass / Fail | | Attach the remaining vial inventory as a continuation sheet using the same fields. # Fixture and identification preflight | Check | Acceptance | Result / evidence | |---|---|---| | Metal cradle location | No glass contact with bath vessel or heater | | | Fixed-stop retainer | Stop dimension recorded; no arbitrary compression | | | Stopper seating | Repeatable installed height | | | Guard and tray | Full fragment/splash interception | | | Above-bath printed parts | PETG only; no hot structural role | | | Hand-tool fallback | Metal fallback documented | | | Cell-wall sensor datum | Marked, dry, repeatable, photographed | | | Cold-spot reserve area | Visible and unobstructed | | | Identifier | Paint/marker plus engraved metal duplicate | | | Webcam | Both displays and clock continuously readable | | | Safe removal | Cell can be handled without forcing stopper | | Preflight disposition: **Pass / Fail / Conditional** Reviewer and date: ______________________________ # Instrument calibration Calibrate the DMM thermocouple and bath thermometer together before the campaign. Record the actual bath condition; do not force either reading to the nominal value. | Point | Reference condition | DMM cell probe | Bath thermometer | Difference | Pass/notes | |---|---|---:|---:|---:|---| | Ice | Stirred ice-water slurry | C | C | C | | | Hot | Stirred hot water, reference temperature recorded | C | C | C | | Cell-probe tape type/lot: ______________________________ Marked bead height: __________ mm from vial bottom Wrap count and width: ______________________________ Placement photograph: ______________________________ # Water-blank preparation Prepare three independent cells, each containing `5.000 +/- 0.005 g` distilled water. Use the same closure process intended for SAT cells. | Cell ID | Empty vial g | Water g | Closed mass g | Stop height mm | PTFE turns | Photo | |---|---:|---:|---:|---:|---:|---| | `WB-1` | | | | | | | | `WB-2` | | | | | | | | `WB-3` | | | | | | | ## Per-cycle run log Use one copy of this table per cell and temperature stage. Record the matching webcam filename and retain the full video. Cell: __________ Stage: **65 C / 80 C** Video: ______________________________ | Cycle | Start | Peak bath C | Peak wall C | Stopper shift | Leakage/condensation | Fault/event time | Pass | |---:|---|---:|---:|---|---|---|---| | 1 | | | | | | | | | 2 | | | | | | | | | 3 | | | | | | | | | 4 | | | | | | | | | 5 | | | | | | | | | 6 | | | | | | | | | 7 | | | | | | | | | 8 | | | | | | | | | 9 | | | | | | | | | 10 | | | | | | | | ## Ten-cycle inspection | Field | Before | After | Change / result | |---|---:|---:|---| | Closed cell mass | g | g | g | | Stopper installed height | mm | mm | mm | | PTFE seam condition | | | | | Glass condition | | | | | Identifier legibility | | | | | Sensor tape condition | | | | Pilot pass requires all three cells to complete ten 25-65 C cycles before any 80 C stage. The 80 C stage is a separate ten-cycle qualification. Reject on: - visible leakage, stopper displacement, glass damage, or uncontrolled heating; - sensor disagreement unexplained by measured lag; - individual ten-cycle mass change greater than 0.02 g; - loss of guard, fixture, tape, identifier, or video integrity. The 0.02 g criterion is a pilot leak screen, not the formal SAT mass-retention gate. # Thermal baseline After water blanks pass, run sequential baselines with identical fixture and sensor placement: 1. empty closed cell; 2. 5.000 g distilled-water cell; 3. 5.000 g pure-SAT cell after stock qualification; 4. `SAT-SEED+` control using the same SAT batch. | Run ID | Contents | Profile | Bath-wall lag | Wall offset | Event visibility | Video | Pass | |---|---|---|---:|---:|---|---|---| | | Empty | | s | C | | | | | | Water | | s | C | | | | | | Pure SAT | | s | C | | | | | | SAT-SEED+ | | s | C | | | | Do not claim a 0.5 C/min profile until measured bath data demonstrate the rate. Document the actual ramp, holds, overshoot, cooling method, wall lag, and ambient conditions. A crystallization event is credited only when the wall transient is distinguishable from the simultaneously recorded bath behaviour. # Formal readiness gates | Gate | Requirement | Status / evidence | |---|---|---| | Incoming inspection | All used vials and closures accepted | | | Fixture | Fit, fixed stop, guard, tray, removal pass | | | Instrumentation | Two simultaneous channels calibrated | | | Logging | Displays and clock continuously readable | | | 65 C blanks | 3/3 cells, 10/10 cycles each | | | 80 C blanks | 3/3 cells, 10/10 cycles each | | | Baselines | Empty, water, pure SAT, SAT-SEED+ characterized | | | Formal weighing | 0.001 g scale available and verified | | | Ramp claim | Actual rate demonstrated or claim withheld | | The formal mass-retention requirement is no more than 0.2% per ten-cycle block, equal to 0.010 g for a 5.000 g specimen. The present 0.01 g scale cannot support a defensible pass at that boundary. Require 0.001 g resolution before marking this gate passed. # Failure, archive, and approval record | Cell ID | Failure or completion | Immediate action | Photo/video | Final disposition | |---|---|---|---|---| | | | | | Archive / open / discard | | | | | | Archive / open / discard | | | | | | Archive / open / discard | Archive representative successful cells intact when storage permits. Record any destructive opening, recovery, breakage, disposal, or inability to archive. Fixture qualification decision: **Approved / Rejected / More evidence required** Authorized variants: **STD / COLD interface only / RSEED interface only** Unresolved limitations: ____________________________________________________ Tristan signature/date: ____________________________________________________ # References - `Chemistry/PCM_Cells/NanoArc_PCM_Test_Cell_Family_Rev0.md` - `Chemistry/SAT/NanoArc_SAT_Crystallization_Route_Plan_Rev0.md` - J. Li, M. A. Parkes, and C. G. Salzmann, *Crystal Growth & Design* 24 (2024), DOI `10.1021/acs.cgd.4c00691`.