Category: Pump

I. Instrument Overview and Basic Operations

1.1 Instrument Introduction

The Thermo Fisher FlashSmart Elemental Analyzer is a fully automated organic elemental analysis system that employs the dynamic combustion method (modified Dumas method) to determine nitrogen, carbon, hydrogen, and sulfur content. It measures oxygen content through high-temperature pyrolysis. This instrument can be configured with a single-channel or dual independent-channel system, and the MultiValve Control (MVC) module enables automatic dual-channel switching for analysis.

Main Technical Parameters:

• Detector Type: Thermal Conductivity Detector (TCD)
• Power Supply: 230V ± 10%, 50/60Hz, 1400VA
• Dimensions: 50cm (height) × 59cm (width) × 58cm (depth)
• Weight: 65kg
• Maximum Operating Temperature: 1100℃
• Gas Requirements: High-purity helium (carrier gas), oxygen (combustion aid), argon (for specific configurations)

1.2 Safety Precautions

Hazardous Operation Warnings:

• High Voltage Risk: The instrument contains high-voltage components. Non-professionals are prohibited from opening the electrical compartment.
• High-Temperature Surfaces: The furnace can reach temperatures up to 1100℃. Avoid contact during operation.
• Gas Safety: Hydrogen use requires extreme caution, as concentrations as low as 4% pose an explosion risk.
• Chemical Hazards: Wear protective gear when handling reaction tube packing materials and sample ashes.

Personal Protective Equipment (PPE) Requirements:

• Eye Protection: Splash-resistant goggles
• Hand Protection: White nitrile gloves (for chemicals)/heat-resistant gloves (for high-temperature operations)
• Respiratory Protection: Dust masks
• Body Protection: Lab coats + plastic aprons

1.3 Startup Preparation Procedure

Gas Connection:

• Helium Inlet Pressure: 2.5bar (36psig)
• Oxygen Inlet Pressure: 2.5-3bar (36-44psig)
• Argon Inlet Pressure: 2.5bar (N/Protein configuration) or 4-4.5bar (NC Soils configuration)
• Leak Testing: Perform on all gas lines.

Power Connection:

• Confirm voltage stability at 230V ± 10%.
• Ensure proper grounding; avoid sharing circuits with large motor equipment.

Software Installation:

• System Requirements: Windows 7/8/10, at least 1GB hard drive space.
• Install EagerSmart data processing software and drivers.

II. Calibration and Adjustment Procedures

2.1 Initial Setup

Hardware Configuration Steps:

• Select Reaction Tube Configuration Based on Analysis Needs:
  • CHN Mode: Quartz reaction tube + chromium oxide/reduced copper/cobalt oxide packing.
  • CHNS Mode: Quartz reaction tube + copper oxide/electrolytic copper packing.
  • O Mode: Quartz reaction tube + nickel-plated carbon/quartz shavings packing.
  • N Mode: Dual reaction tubes in series + Plexiglas adsorption filter.
• Install Autosampler:
  • MAS Plus Solid Autosampler: Up to 125-position sample tray.
  • AI 1310/AS 1310 Liquid Autosamplers: 8-position or 105-position sample trays.
• Connect MVC Module (Dual-Channel Configuration):
  • Remove bypass panel from the rear.
  • Connect gas lines for left and right channels.
  • Configure dual MAS Plus autosamplers.

2.2 System Calibration

Three-Step Calibration Method:

• Leak Testing:
  • Initiate automatic leak detection via software.
  • Acceptable Leak Rate: <0.1mL/min.
  • Use soapy water to locate leaks if detected.
• Signal Baseline Adjustment:
  • Set TCD detector temperature constant (typically 40-120℃).
  • Adjust bridge voltage to 5V.
  • Baseline Drift: Should be <0.1mV/10min.
• Standard Curve Establishment:
  • Use high-purity standards like acetanilide (nitrogen 16.09%, carbon 71.09%, hydrogen 6.70%).
  • Minimum Concentration Gradients: 5 points (recommended range: 0.1-5mg).
  • Correlation Coefficient (R²): Should be >0.999.

Calibration Frequency Recommendations:

• Daily Use: Calibrate after each startup.
• Continuous Analysis: Verify calibration every 50 samples.
• After Consumable Replacement: Recalibration is mandatory.

2.3 Method Optimization

Parameter Adjustment Guidelines:

• Oxygen Injection Time:
  • Regular Samples: 4-6 seconds.
  • Refractory Samples: Extend to 8 seconds.
  • High-Sulfur Samples: Add vanadium pentoxide as a combustion aid.
• Furnace Temperature Settings:
  • Combustion Furnace: 950-1100℃.
  • Reduction Furnace: 840℃.
  • Pyrolysis Furnace (O Mode): 1060℃.
• Carrier Gas Flow Rate:
  • Helium: 100-140mL/min.
  • Reference Gas: 30-50mL/min.

III. Routine Maintenance

3.1 Regular Maintenance Schedule

Maintenance Schedule Table:

Maintenance Item	Frequency	Key Operation Points
Reaction Tube Regeneration	Every 200 analyses	Empty packing material, incinerate at 550℃ for 2 hours.
Adsorbent Replacement	Monthly	Activate molecular sieve at 300℃, replace desiccant (silica gel) promptly.
Autosampler Cleaning	Weekly	Ultrasonically clean tin/silver cups, inspect piston seals.
Chromatographic Column Aging	Quarterly	Age at 280℃ with carrier gas for 8 hours.
Comprehensive System Verification	Annually	Conducted by a professional engineer.

3.2 Key Component Maintenance

Reaction Tube Packing Guidelines:

• Quartz Reaction Tubes:
  • Begin packing from the conical end.
  • Compact each layer with a dedicated tamping rod.
  • Separate layers with quartz wool.
  • Maintain total packing height at 80% of tube length.
• HPAR Alloy Steel Reaction Tubes:
  • Must be used with crucibles.
  • Ensure uniform distribution of oxidation catalysts.
  • Use dedicated tools for installation/removal.

Adsorption Filter Maintenance:

• Large (Plexiglas) Filters:
  • Packing sequence: Quartz wool → soda lime → molecular sieve → silica gel.
  • Pre-moisten soda lime with 0.5mL water.
• Small (Pyrex) Filters:
  • Used in CHNS/O modes.
  • Packing: Quartz wool → anhydrous magnesium perchlorate.

3.3 Consumable Replacement Intervals

Recommended Replacement Intervals:

• Quartz Wool: Replace when changing reaction tube packing.
• Reduced Copper: Every 500 analyses.
• Oxidation Catalyst: Every 300 analyses.
• Nickel-Plated Carbon (O Mode): Every 150 analyses.
• TCD Filament: Replace when baseline noise occurs.
• Sealing O-Rings: Replace if leaks are detected or every 6 months.

IV. Troubleshooting and Solutions

4.1 Common Error Codes

Error Code Table:

Code	Meaning	Solution
E01	Left Furnace Temperature Exceeded	Check thermocouple connection, restart system.
E04	TCD Signal Overflow	Adjust gain, verify carrier gas purity.
E12	Safety Cutoff Triggered	Check cooling fan, allow system to cool.
E25	EFC-t Module Flow Abnormality	Check for gas line blockages, clean filter.
E33	Autosampler Communication Failure	Reconnect cables, verify port settings.

4.2 Typical Problem Resolution

Analysis Result Anomaly Investigation:

• Low Nitrogen Results:
  • Check if reduced copper is失效 (discolored black).
  • Verify adequate oxygen injection.
  • Confirm complete sample combustion (observe flame).
• Sulfur Peak Tailings:
  • Replace copper oxide packing layer.
  • Add vanadium pentoxide combustion aid.
  • Check chromatographic column connections for leaks.
• Unstable Oxygen Results:
  • Verify nickel-plated carbon packing height (should be 60mm).
  • Confirm silver cup seal integrity.
  • Validate pyrolysis furnace temperature stability (±2℃).

Hardware Fault Handling:

• Furnace Temperature Failure to Rise:
  • Check SSR solid-state relay status.
  • Measure transformer output voltage (should be 48V AC).
  • Confirm fuse integrity (AC 1112 board F1/F2).
• Abnormal Gas Flow:
  • Clean EFC-t module filter.
  • Verify solenoid valve EV1-EV4 operation.
  • Calibrate flow sensors S1/S2.
• TCD Baseline Drift:
  • Extend equilibration time to 2 hours.
  • Verify reference gas flow stability.
  • Replace aged filament.

4.3 Emergency Response Procedures

Safety Emergency Plan:

• Gas Leak:
  • Immediately close cylinder main valve.
  • Activate laboratory ventilation system.
  • Avoid operating electrical equipment.
• Furnace Overheating:
  • Trigger front panel emergency stop button.
  • Cut off main power supply.
  • Purge system with inert gas.
• Abnormal Combustion:
  • Maintain system enclosure.
  • Direct exhaust through fume hood.
  • Do not cool directly with water.

V. Advanced Application Techniques

5.1 Special Sample Handling

Solutions for Challenging Samples:

• High Inorganic Salt Samples:
  • Use quartz crucibles to prevent corrosion.
  • Reduce quartz wool between packing layers.
  • Increase oxygen injection pressure by 10%.
• Volatile Liquids:
  • Utilize AI 1310 liquid autosampler.
  • Adsorb sample onto diatomaceous earth.
  • Preheat injection needle to 40℃.
• Viscous Samples:
  • Grind with quartz sand for homogenization.
  • Use specially shaped tin cups.
  • Extend combustion time by 20%.

5.2 Data Quality Enhancement

Best Practice Recommendations:

• Sample Preparation:
  • Homogenize to below 80 mesh.
  • Pre-dry samples with >5% moisture content.
  • Avoid fluorine-containing containers.
• Weighing Techniques:
  • Use blank tin cups for calibration with microsamples (<1mg).
  • Employ “sandwich” loading method for highly volatile samples.
  • Utilize a 0.1μg precision balance.
• Quality Control:
  • Insert standard samples every 10 analyses.
  • Maintain parallel sample deviation <1.5%.
  • Retain all original chromatograms.

5.3 Automation Features

Intelligent Function Applications:

• Standby Mode:
  • Reduce carrier gas to 10mL/min.
  • Maintain furnace temperature at 50% of setpoint.
  • Auto-wake via timer function.
• Sequence Analysis:
  • Supports 125-sample unattended operation.
  • Enables alternating method runs.
  • Auto-generates comprehensive reports.
• Remote Monitoring:
  • View system status remotely via EagerSmart software.
  • Set up email alerts.
  • Auto-backup data to network.

VI. Appendices and Support

6.1 Technical Specifications Summary

Key Parameter Quick Reference Table:

• Detection Limits: N/C/H 0.01%, S/O 0.02%
• Precision: RSD <0.5% (for conventional elements)
• Analysis Time: CHN 5min, O 4min, CHNS 6min
• Sample Size: 0.01-100mg (solid), 0.1-10μL (liquid)
• Gas Consumption: Approximately 10L helium per sample

6.2 Regulatory Compliance

Certifications and Compliance:

• CE Certification: Complies with EN 61010-1 safety standards.
• RoHS: Complies with Directive 2011/65/EU.
• WEEE: Classification number 23103000.
• GLP/GMP Compliance: Meets regulatory requirements.

This guide is based on the FlashSmart Elemental Analyzer Operating Manual (P/N 31707001, Revision E) and covers key points for the instrument’s operational lifecycle. Always adapt usage to specific configurations and application needs while strictly adhering to local safety regulations.