Synthesis System

The synthesis system automates solid-state reactions and includes:

• Chemspeed Swing XL Synthesizer – controlled via programmable input files
  • Ball mill for precursor mixing
  • Pellet press for compaction
  • Furnace with programmable temperature profiles

Each system is represented as an ssn:System or subclass, deployed via ssn:Deployment.

Analytical Systems

Post-synthesis, materials are analyzed using:

• Malvern-Panalytical Aeris Benchtop XRD (X-ray Diffraction) – for phase identification
• Advion Avant UHPLC with CMS – for impurity profiling
• Agilent 8990 GC + Hiden QGA MS -
• TGA-SDT650 – for thermal decomposition and mass loss profiling
• Electrochemical Workstation (Biologic SP-200) – for voltage, current, and conductivity measurements
• Liquid-Liquid Separation Platform (J-Kem) -

Each instrument is modeled as an ssn:System capable of generating one or more sosa:Observations.

Sample Handling and Transport

• KUKA Robotic Arm – handles sample manipulation within stations.
• KUKA Mobile Robot – transports samples between synthesis and analytical stations. Each is tracked as an :rdfterm and supports associated :rdfterms for movement and handoff.

Chemspeed SwingXL

A programmable synthesis platform with solid and liquid dispensing down to 0.1 mg precision. Includes:

• Gravimetric dispensing
• Overhead reaction control (heating, cooling, stirring, reflux, pH monitoring/titration)
• ISYNTH disposable glass reactor blocks
• High-temp annealing furnace

Advion Avant UHPLC with CMS

Advanced LC system with autosampler, dual MTP trays, and multiple detection modes:

• UV/Vis and RI detectors
• Compact Mass Spectrometer (CMS, electrospray)
• Column oven up to 90°C and pressure support up to 18,850 psi
• Manual or robotic injection from SwingXL or sample trays

Agilent 8990 GC + Hiden QGA MS

Gas chromatography unit with dual columns and thermal conductivity detectors (TCD):

• Ar and He carrier gas configurations
• In-line catalytic reactor compatibility
• Optional Hiden QGA MS for product ID (low detection limits)

Malvern-Panalytical Aeris Benchtop XRD

Cu Kα X-ray diffraction system for solid phase identification:

• Supports automated sample handoff from SwingXL
• Suitable for phase ID and structure refinement

Electrochemical Workstation (Biologic SP-200)

Integrated into a custom J-Kem catalytic station:

• Measures electrochemical response for electrocatalytic CO₂ conversion
• Compatible with single or H-cell reactors
• Automates electrolyte/gas control and temperature logging

TA Instruments SDT-650 (TGA/DSC-MS)

Thermogravimetric and differential scanning calorimetry system:

• Operates to 1500°C in inert/oxidizing/reducing atmospheres
• Supports modulated TGA/DSC
• Pfeiffer MS extension for evolved gas analysis up to 300 AMU

Liquid-Liquid Separation Platform (J-Kem)

Automated workflow for selective phase extraction:

• Ligand-controlled solvation studies
• Weighing, centrifugation, imaging, and spectral quantification

Step 1: Sample Synthesis

1. Mix precursors (acl:PrecursorMixture)
2. Grind in Mill
3. Compact into pellet (optional)
4. Fire in furnace
5. Grind in Mill (repeat 2-4) (optional, as needed for purity)
6. Result: acl:SolidSample

acl:run123 a prov:Activity ;
  prov:used acl:precursorMixture456 ;
  prov:generated acl:sample789 ;
  prov:wasAssociatedWith acl:automatedFurnace ;
  prov:startedAtTime "2025-07-10T09:00:00Z"^^xsd:dateTime .

Step 2: Sample Analysis

1. Load sample on zero background XRD holder
2. Load holder with sample on XRD
3. Collect diffraction pattern
4. Derive acl:phaseStructure, acl:phaseComposition, acl:purity

acl:xrdObs123 a sosa:Observation ;
  sosa:hasFeatureOfInterest acl:sample789 ;
  sosa:observedProperty acl:phaseComposition ;
  sosa:madeBySensor acl:XRDSystem ;
  sosa:resultTime "2025-07-10T12:15:00Z"^^xsd:dateTime ;
  sosa:hasResult [
    rdf:value "Orthorhombic perovskite" ;
    qudt:unit qudt:Dimensionless
  ] .

Other measurements (HPLC, ICP-OES, FTIR, Ramman, UV-VIS, TGA) follow a similar pattern.

Synthesis Input

XRD Analysis Outputs

TGA Analysis Outputs

HPLC Analysis Outputs

Each store is independently addressable and associated with a :rdfterm[dcat:DataService], for example:

acl:xrdRawService a dcat:DataService ;
  dct:title "XRD XRDML Store" ;
  dcat:endpointURL <https://data.example.org/minio/acl-xrd-xrdml/> ;
  dcat:servesDataset acl:xrdDataset .