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Hardware Setup Guide

Complete guide for setting up and configuring SIA-CE hardware components.

System Requirements

Computer Requirements

Minimum: - Windows 7 SP1 (64-bit) - 4 GB RAM - 2.0 GHz processor - 10 GB free disk space - 2 available USB/Serial ports

Recommended: - Windows 10/11 (64-bit) - 8 GB RAM or more - 3.0 GHz multi-core processor - 50 GB free disk space - Dedicated USB ports (not hub)

Software Requirements

  • Agilent ChemStation (version B.04.03 or higher)
  • Python 3.7+ (64-bit recommended)
  • Required Python packages (see installation guide)

CE System Setup

Agilent 7100 CE System

Initial Setup

  1. Power Connection
  2. Connect to appropriate voltage (100-240V)
  3. Use surge protector
  4. Ensure proper grounding

  5. Communication

  6. Connect USB cable to PC
  7. Install ChemStation drivers
  8. Configure in ChemStation

  9. Capillary Installation

  10. Use proper capillary cutting tool
  11. Check window alignment
  12. Verify detection path

Configuration in ChemStation

1. Open ChemStation
2. Go to Instrument → Configure
3. Select CE instrument
4. Set communication parameters:
   - Connection: USB
   - Timeout: 30 seconds
5. Test connection

Vial Positions: - Positions 1-48: Sample vials - Position 49: Replenishment parking - Position 50: Often used for waste

Vial Types: - 100 µL microvials (recommended for small volumes) - 1 mL polypropylene vials - 2 mL glass vials

Best Practices: - Use same vial type throughout analysis - Check vial seating in carousel - Replace damaged carousel positions

SIA System Setup

Syringe Pump Installation

Hamilton MVP Series

  1. Physical Setup

    - Mount on stable surface
    - Level the pump
    - Install syringe (finger-tight only)
    - Connect valve assembly
    

  2. Electrical Connection

    - Connect power supply (12-24V DC)
    - Connect RS-232 cable to PC
    - Set DIP switches if required
    

  3. Communication Settings

    Port: COM3 (typical)
    Baud: 9600
    Data bits: 8
    Stop bits: 1
    Parity: None
    Flow control: None
    

Syringe Selection

Volume Range Syringe Size Resolution Best For
10-100 µL 100 µL 0.03 µL Precise small volumes
50-500 µL 500 µL 0.17 µL General use
100-1000 µL 1000 µL 0.33 µL Standard operations
500-5000 µL 5000 µL 1.67 µL Large volume prep

Valve Selector Installation

VICI/Valco Setup

  1. Mounting

    - Secure to stable platform
    - Align ports horizontally
    - Minimize tubing lengths
    

  2. Port Connections

    Port 1: Waste
    Port 2: Air/Gas
    Port 3: DI Water
    Port 4: Transfer to CE
    Port 5-8: Reagents/Solvents
    

  3. Communication

    Port: COM4 (typical)
    Baud: 9600
    Protocol: VICI standard
    

Tubing and Connections

Tubing Selection

Application ID (mm) Material Length
Syringe-Valve 0.8 PTFE < 10 cm
Valve-Ports 0.5 PEEK < 30 cm
To CE 0.25 Fused Silica < 50 cm
Waste 1.6 PTFE As needed

Connection Best Practices

  1. Cutting Tubing
  2. Use sharp blade
  3. Cut perpendicular
  4. No burrs or deformation

  5. Fittings

  6. Finger-tight + 1/4 turn
  7. Use appropriate ferrules
  8. Check for leaks

  9. Dead Volume

  10. Minimize connection volume
  11. Use zero-dead-volume fittings
  12. Flush after installation

System Integration

Physical Layout

Recommended Setup:
┌─────────────┐     ┌──────────┐
│   CE System │     │ Computer │
│             │────>│          │
└─────────────┘     └──────────┘
       ^                  ^
       │                  │
┌──────┴─────┐     ┌─────┴────┐
│   Syringe  │────>│  Valve   │
│    Pump    │     │ Selector │
└────────────┘     └──────────┘

Communication Architecture

  1. Serial Ports

    # Find available ports
    import serial.tools.list_ports
    
    ports = serial.tools.list_ports.comports()
    for port in ports:
        print(f"{port.device}: {port.description}")
    

  2. Port Assignment

  3. Use Device Manager to identify
  4. Assign consistent port numbers
  5. Document port mapping

Power Management

  1. Power Sequence

    1. Computer
    2. CE System
    3. Syringe Pump
    4. Valve Selector
    

  2. UPS Recommendations

  3. Minimum 1000 VA
  4. Include all components
  5. Test monthly

Calibration and Testing

Syringe Pump Calibration

def calibrate_syringe_volume():
    """Calibrate syringe volume delivery."""

    # Initialize
    syringe.initialize()

    # Test volumes
    test_volumes = [100, 500, 900]

    for volume in test_volumes:
        # Dispense into tared vial
        syringe.aspirate(volume)
        input(f"Place tared vial at output. Press Enter...")
        syringe.dispense(volume)

        actual = float(input("Enter measured volume (µL): "))
        error = (actual - volume) / volume * 100
        print(f"Volume: {volume} µL, Error: {error:.2f}%")

Valve Position Verification

def verify_valve_positions():
    """Verify each valve position."""

    num_positions = 8

    for pos in range(1, num_positions + 1):
        valve.position(pos)
        input(f"Verify position {pos}. Press Enter...")

    print("Valve verification complete")

CE System Tests

  1. Pressure Test

    # Test pressure system
    api.ce.apply_pressure_to_capillary(50, 10)  # 50 mbar, 10 sec
    api.ce.apply_pressure_to_capillary(-50, 10)  # -50 mbar, 10 sec
    

  2. Carousel Test

    # Test all positions
    for pos in range(1, 49):
        try:
            api.ce.load_vial_to_position(pos, "inlet")
            api.ce.unload_vial_from_position("inlet")
            print(f"Position {pos}: OK")
        except:
            print(f"Position {pos}: FAIL")
    

Maintenance Schedule

Daily

  • Check for leaks
  • Verify communication
  • Clean needle/transfer line

Weekly

  • Flush all lines
  • Check capillary condition
  • Calibrate if needed

Monthly

  • Deep clean system
  • Replace worn tubing
  • Check electrical connections

Annually

  • Service syringe pump
  • Replace seals
  • Full system validation

Troubleshooting

Communication Issues

Problem: COM port not found

Solution:
1. Check Device Manager
2. Reinstall drivers
3. Try different USB port
4. Use USB-Serial adapter if needed

Problem: Device not responding

# Test communication
try:
    syringe.send_command("?", get_response=True)
    print("Syringe communication OK")
except:
    print("Check connections and power")

Mechanical Issues

Problem: Syringe stalling

Causes:
- Overpressure
- Mechanical binding
- Wrong syringe size configured

Solutions:
- Check for blockages
- Reduce speed
- Verify syringe size setting

Problem: Valve not switching

Causes:
- Mechanical obstruction
- Communication error
- Power issue

Solutions:
- Manual rotation check
- Increase switching attempts
- Check power supply

System Integration Issues

Problem: Timing conflicts

# Add delays between operations
def safe_operation_sequence():
    valve.position(1)
    time.sleep(0.5)  # Allow valve to settle
    syringe.aspirate(500)
    time.sleep(0.2)  # Allow pressure to stabilize

Optimization Tips

Speed Optimization

  1. Parallel Operations
  2. Prepare next sample during CE run
  3. Use continuous flow for same solvent
  4. Minimize valve switches

  5. Flow Rates

    # Optimized speeds
    SPEEDS = {
        'air': 5000,        # Fast
        'water': 3500,      # Medium-fast
        'organic': 2500,    # Medium
        'viscous': 1000,    # Slow
        'critical': 500     # Very slow
    }
    

Volume Optimization

  1. Minimize Dead Volume
  2. Short tubing runs
  3. Small ID tubing where possible
  4. Zero-dead-volume fittings

  5. Efficient Aspiration

    # Aspirate in order of reactivity
    # 1. Buffer/diluent (least reactive)
    # 2. Sample (most reactive)
    # 3. Air gap (separation)
    

Reliability Enhancement

  1. Error Recovery

    # Implement retry logic
    def reliable_operation(func, retries=3):
        for attempt in range(retries):
            try:
                return func()
            except:
                if attempt == retries - 1:
                    raise
                time.sleep(1)
    

  2. State Monitoring

    # Track system state
    class SystemMonitor:
        def __init__(self):
            self.syringe_volume = 0
            self.valve_position = 1
            self.last_operation = None
    

Safety Considerations

Chemical Safety

  • Use fume hood for volatile solvents
  • Proper waste disposal
  • Material compatibility checks

Electrical Safety

  • Proper grounding
  • No liquid near electronics
  • Emergency stop procedures

Pressure Safety

  • Maximum 100 mbar for injection
  • Maximum 950 mbar for flushing
  • Pressure relief mechanisms

Validation Protocols

IQ/OQ/PQ

  1. Installation Qualification (IQ)
  2. Document all connections
  3. Verify communication
  4. Check safety features

  5. Operational Qualification (OQ)

  6. Test all functions
  7. Verify accuracy
  8. Document performance

  9. Performance Qualification (PQ)

  10. Run test methods
  11. Verify reproducibility
  12. Meet specifications

Setup Complete

With proper hardware setup, your SIA-CE system is ready for automated analysis!