The ChromasterUltra RS 6430 Diode Array Detector is a high-performance liquid chromatography (HPLC) detector designed for research use. It is not intended for patient diagnostic or therapeutic results. This instruction manual provides comprehensive details on its operation, maintenance, and safety precautions.
Function Description
The ChromasterUltra RS 6430 Diode Array Detector is a key component of the ChromasterUltra RS System, which performs liquid chromatography to separate and detect substances in a sample. The detector unit is responsible for detecting separated sample components as electric signals.
Key features of the ChromasterUltra RS 6430 include:
- High Transmittance Flow Cell Based on Total Reflection: To achieve high light transmittance and a small cell volume suitable for UHPLC applications, a silica glass capillary flow cell is employed. Incident light is reflected at the boundary between the capillary wall and outer air without loss, similar to an optical fiber, ensuring high light intensity through the narrow flow path.
- Thermostated Light Source Unit: The light source unit is cooled by Peltier temperature control, maintaining an optimal D2 lamp temperature regardless of environmental conditions.
- High Speed Data Sampling Rate: The detector boasts a data sampling rate of 10 msec, sufficient for various UHPLC applications.
- Easy Wavelength Accuracy Check: An Hg lamp is integrated for automatic wavelength accuracy checks of the optical system, requiring no additional preparation or settings.
- Easy Maintenance: All periodic replacement parts are accessible from the instrument's front panel, simplifying maintenance procedures.
The optical system of the detector works by condensing light emitted from a D2 lamp into the flow cell unit via a condensing mirror. This incident light enters a capillary flow cell through an incident-side optical fiber. Light transmitted through the sample in the flow cell exits via an emission-side optical fiber, is condensed at the spectrometer's incident slit, and then enters the spectrometer. Inside the spectrometer, the light is dispersed by a grating and converted into an electric signal by a photodiode array (PDA). For wavelength accuracy checks, light from the D2 lamp is blocked, and light from the Hg lamp is reflected into the spectrometer.
Important Technical Specifications
- Optical System: Single beam photometric system (dispersion by diffraction grating).
- Light Source: D2 lamp, Hg lamp (for wavelength check).
- Detecting Element: 1024-bit photodiode array.
- Measuring Wavelength Range: 190 to 650 nm.
- Spectrum Bandwidth: 1, 2, 4, 8, 16 nm.
- Wavelength Setup: Via CDS or GUI controller.
- Wavelength Accuracy: ±1 nm.
- Slit Type: Two settings; FINE (<1 nm>), COARSE (<4 nm>).
- Time Constant: Selectable in 7 steps (0.01, 0.02, 0.05, 0.1, 0.5, 1.0, 2.0 sec).
- Noise: Within 0.5 × 10⁻⁵ AU (measured with standard flow cell, methanol at 0.5 ml/min, COARSE slit, bandwidth 4 nm, smoothed chromatogram 250 ± 10 nm, reference 360 nm ± 50 nm, sampling period 400 ms, response 2 s, ambient temperature variation within 2 °C (20 to 30°C), after 1 hr warm-up).
- Drift: Within 0.4 × 10⁻³ AU/h or 0.4 × 10⁻³ AU/h/°C, whichever is greater (measured under similar conditions as noise, but with sampling period 1600 ms).
- Linearity: 2.0 AU (5 %) (acetone, 250 nm).
- Communication Function: e-Line (instrument conditions, instrument status), USB2.0 (accumulated data).
- External Input/Output Contact Terminals: START IN, ERROR IN, ERROR OUT, BUSY OUT (contacts on e-Line).
- Flow Cell: Standard flow cell (optical path length 10 mm, cell capacity 2.2 µL), High sensitivity flow cell (option) (optical path length 65 mm, cell capacity 14 µL).
- Wetted Part Material: Fluorine resin, PEEK resin, Quartz glass, SUS316.
- Flow Cell Withstand Pressure: 6.0 MPa.
- Operating Temperature Range: 15 to 35 °C (non-condensing).
- Operating Humidity Range: 25 to 85 % (non-condensing).
- Power Source: AC 100 to 240 V ± 10 % (50 / 60 Hz).
- Power Consumption: 160 VA.
- Outer Dimensions: 340 mm (W) × 515 mm (D) × 153 mm (H).
- Weight: 17 kg.
- Confidence Functions: Used with Chromato Data Station (CDS) or GUI controller for wavelength accuracy check (D2 lamp emission lines at 486 mm and 656 mm; Hg lamp bright lines at 254 mm, 365 mm, 436 mm, 546 mm), and recording of lighting time, number of times, and replacement dates for D2 and Hg lamps.
Usage Features
The detector's operation is primarily controlled and managed via the Chromatography Data Station (CDS) software installed on a PC. This includes data acquisition parameters, photometric values, and error information. Three-dimensional data acquisition allows for real-time monitoring of contour maps, spectra, and chromatograms on the PC. After analysis, this data is stored on the PC's hard disk or a network database, enabling peak purity checks, component identification, and library data creation/search.
Power-On: The instrument is turned on via the main switch. LEDs indicate power status (blue for ON, orange for ERROR), analysis status (RUN, blue), lamp house temperature (TEMP, blue), and D2 lamp status (D2 LAMP, blue for ON, off for OFF). If an error occurs, refer to the troubleshooting section.
Cautions on Operation:
- Solvent Selection: Use solvents with very low UV absorption for high-sensitivity analysis. Be aware that absorption characteristics vary between production lots and manufacturers for high-grade reagents like methanol, ethanol, or acetonitrile, especially at short wavelengths.
- Flow Cell Life: The quartz capillary in the flow cell can degrade due to UV exposure, shortening its lifespan, particularly with low UV absorption mobile phases (e.g., acetonitrile or water). It is recommended to turn off the light source lamp after analysis to slow degradation.
- Mobile Phase Restrictions: The wetted parts of the flow cell use PEEK resin and SUS316. Avoid solvents or reagents that can corrode or swell these materials (e.g., tetrahydrofuran, dichloromethane, chloroform, acetone, dimethylsulfoxide, or solutions containing halide ions like HCl, KCl, NaCl, NH4Cl).
- Washing the Flow Cell: After using unsuitable reagents or buffer solutions, thoroughly wash the flow paths with an appropriate solvent (e.g., methanol or acetonitrile for organic mobile phases, distilled water for aqueous solutions). Failure to wash can lead to clogging or damage.
- Flow Cell Storage: When not in use, keep the flow cell filled with distilled water or alcohol. For long-term storage (over 1 month), fill it with isopropanol. Do not allow the flow line to dry out, as this can cause baseline instability.
- High Pressure: The system operates under high pressure, and chemicals may spurt. Wear protective eyewear when using toxic solvents.
- Fatigue: Take regular breaks (10-15 minutes per hour) when working with the display monitor and keyboard for extended periods to prevent eye and body fatigue.
Shutdown: Turn off the instrument's power switch. For the CDS, shut down the PC first. Measurement parameters are saved even when power is off and will be recalled upon restart.
Maintenance Features
The manual outlines periodic checkups and maintenance procedures to ensure reliable operation and prevent issues.
Confirmation of Basic Actions:
- Ensure the instrument is installed correctly (refer to Appendix 1).
- Turn on the detector's power switch and confirm the "POWER" LED is on.
- Confirm the "D2 LAMP" is lit.
- Start CDS and verify the diode array detector is in "Ready" status.
Confirmation of Performance Specifications:
- Performance checks should be conducted in a stable environment (room temperature 20-30 °C, variation within 2 °C, no direct airflow from air-conditioners).
- Warm up the instrument for at least 1 hour.
- Use a standard flow cell. If contaminated, clean it before checking performance.
- Wavelength Accuracy: Measure using CDS maintenance software or GUI, targeting D2 lamp lines (486 nm, 656 nm) and Hg lamp lines (254 nm, 365 nm, 436 nm, 546 nm). Accuracy should be within ±1 nm.
- Lamp Energy: Measure D2 lamp energy using CDS maintenance software for both Fine and Coarse slit settings. Estimated energy levels are 1200 or more (Fine) and 12000 or more (Coarse) at 250 nm with a test cell or water-filled standard flow cell.
- Noise/Drift: Measure noise and drift at 250 nm using CDS (EZChrom or Empower). Noise should be 0.5 × 10⁻⁵ AU or less. Drift should be 0.4 × 10⁻³ AU/hr or less, or 0.4 × 10⁻³ AU/hr/°C or less.
Periodic Checkup (Table 5-1):
- Lighting of Lamp: Daily check that "D2 LAMP" LED is lit.
- Liquid Leak: Daily visual check for leaks from mobile phase bottles, tubes, and waste solution.
- Drain Tray: Daily check for contamination. Clean if dust or contaminants are present to prevent leak sensor malfunction.
- Life of Light Source Lamp: Monthly check for poor energy or significant baseline fluctuations to determine if the lamp has reached the end of its service life.
- Leak Sensor: Monthly drip water on the sensor to confirm "LAMP OFF BY LEAKAGE" error occurs, then wipe off water. Visually check for leaks before each measurement.
- Wavelength Accuracy: Yearly check using Hg and D2 lamp bright lines.
Checking and Cleaning the Flow Cell (5.4.1):
- If lamp energy does not recover after D2 lamp replacement, clean the flow cell.
- Deliver detergent into the flow cell with a pump at a low flow rate (0.5 mL/min or lower) and pressure (6.0 MPa or lower).
- Loosen thumbscrews to detach the front lid and then the flow cell clamping screws to separate the flow cell unit.
- Visually inspect the light inlet and outlet for contamination. Wipe with a lens cleaning paper or cotton swab moistened with methanol.
- Reinsert the flow cell unit, aligning with the fix blocks.
Registration of Flow Cell Unit (5.5):
- When replacing the flow cell unit, register its serial number and code using the CDS maintenance software under the "DAD Meta Parameters" screen.
Lamp Replacement (5.7):
- Safety: Always turn off the power switch and unplug the power cord before detaching the light source cover to prevent electric shock. The lamp and cover are hot; wait at least one hour for them to cool before replacement to prevent burns. Do not defeat the safety mechanism that automatically turns off power when the lamp cover is detached.
- D2 Lamp Replacement (5.7.1): Requires a new D2 lamp. Detach the front lid and D2 lamp lid by removing thumbscrews. Disconnect the D2 lamp connector and remove fastening screws to detach the D2 lamp cover. Pull out the old D2 lamp, mount the new one aligning the notch on the flange with the alignment pin. Pass the lead wire through the D2 lamp cover opening and fasten the cover. Secure the lead wire with the fastening band. Connect the lead wire connector to the instrument. Insert the folded wire into the lamp house space. Reattach the D2 lamp lid and front lid. Perform an operation check, warm up for 1 hour, and check lamp energy via CDS. Reset cumulative lamp-on time and count.
- Hg Lamp Replacement (5.7.2): Requires a new Hg lamp unit and a Phillips screwdriver. Ensure power is off and unplugged. Detach the front lid, D2 lamp lid, and Hg lamp lid. Disconnect the Hg lamp unit's lead wire connector from the lamp inverter. Loosen the Hg lamp unit fixing screw and separate the Hg lamp cover. Pull out the old Hg lamp unit. Fit the new Hg lamp unit, attach the Hg lamp cover, connect the lead wire, and reattach the Hg lamp lid and D2 lamp lid. Perform an operation check, start maintenance software, and check the Hg lamp spectrum for a sharp peak near 253.7 nm. Reset cumulative lamp-on time and count.
Fuse Replacement (5.8):
- Safety: Turn off the power switch and unplug the power cord.
- Requires a new fuse (P/N: J821399) and a flat-blade screwdriver.
- Pull out the fuse holder with a flat-blade screwdriver.
- Replace existing fuses and insert the holder back in place.
Accessories (7.1):
- Standard flow cell (P/N: 889-0810) includes a loop tube and light inlet/outlet caps.
- High sensitivity flow cell (option, P/N: 889-0811) also includes a loop tube and light inlet/outlet caps.
- The transmittance of quartz in flow cells degrades due to UV exposure, giving them a finite lifespan. Degradation rate depends on lamp light irradiation time, intensity, and solvent used. The ChromasterUltra RS series has an automatic light extinction function to reduce lamp light irradiation time after analysis.
Safety Summary:
The manual emphasizes reading all safety instructions and precautions, including those on warning labels and in the manual. It defines WARNING (death or serious injury), CAUTION (minor or moderate injury), and NOTICE (property damage) signal words. Users are advised to only perform operations described in the manuals, contact service for issues, and use common sense. Specific warnings include:
- General Safety: Turn off power and disconnect if abnormal conditions (noise, odor, fumes) occur. Do not open laser device panels.
- Flammable Chemicals: The instrument is not explosion-proof. Avoid organic solvents with ignition points below 70 °C in unattended operation. Ensure good ventilation, check for leaks, and use conductive containers with proper grounding to prevent static electricity.
- Explosion of Vapor: Adequate ventilation is crucial when using flammable chemicals to prevent vapor concentration from reaching explosion limits.
- Electric Shock: Turn off power and disconnect the cord before replacing parts like lamps or fuses. Do not open instrument covers. Ensure proper grounding with the supplied 3P power cable or a grounded adapter.
- Toxic/Corrosive/Stimulative Solvents: Wear protective clothing (e.g., safety goggles) and ensure adequate ventilation to prevent skin contact or inhalation. Refer to Safety Data Sheets (SDS).
- Needle/Internal Mechanism Injury: Do not touch the inside of the autosampler during operation.
- Remover Tool Injury: Use care with remover tools when removing plunger seals, wash seals, and guides.
- Xenon Lamp Explosion: Replace xenon lamps before their guaranteed useful lifetime (500 hours for 150 W, 1000 hours for long-life) to prevent explosion due to increased internal pressure. Allow lamps to cool for at least one hour before replacement. Handle lamps with protective gear (safety goggles, mask, thick gloves) to prevent injury from glass pieces if the lamp shatters. Do not apply excessive force to the glass bulb when mounting. Mount the lamp in the specified direction (anode mark aligned with support metal) to prevent excessive cathode consumption and potential explosion. Ensure nuts on the lamp base and wiring are securely tightened to prevent overheating. For disposal, wrap used xenon lamps in thick cloth and crush them to release high-pressure gas before discarding as dangerous waste.
- Heavy Instrument: Modules like the ChromasterUltra RS Organizer (9 kg), 6170 Binary Pump (30 kg), 6270 Autosampler (29 kg), 6310 Column Oven (25 kg), 6420 UV-VIS Detector (15 kg), 6430 Diode Array Detector (17 kg), and 6440 FL Detector (26 kg) are heavy. Handle with care and hold firmly to prevent injury.
- Instrument Tipover: Secure the instrument to prevent accidental tipping.
- Burns: Column ovens, lamps, and lamp covers become hot during operation and remain hot after power-off. Allow sufficient cooling time before contact or replacement.
- Eye Damage: Do not look directly at the illuminating xenon lamp, as it emits intense ultraviolet light. Wear tinted safety glasses.
Installation (Appendix 1):
- Installation should be done by qualified service personnel.
- Transport Screws: Remove transport fixed plates and screws from various modules (Autosampler, DAD, FL Detector, UV-VIS Detector) during installation. Keep these screws for future relocation.
- Power Supply: Requires 100-240 V AC (±10%), 50/60 Hz (±0.5 Hz), 1100 VA or more capacity. Requires five or more grounded 3-pole power outlets.
- Grounding: Ensure proper grounding connection (100 Ω or less resistance) using the supplied 3P power cable.
- Installation Space: Minimum 735 mm wide, 765 mm deep, with 150 mm clearance behind and 100 mm on sides of units. A level, sturdy bench capable of supporting 150 kg or more is required.
- System Tubing: Detailed diagrams and part numbers are provided for connecting various tubes (inlet, drain, flexible) between modules.
- Fastening: Component units are fastened together using fastening plates and screws to prevent tipping.
Contact Signal Communication (Appendix 2):
- The system uses e-Line connectors for contact signals (START, ERROR, BUSY) for common input/output functions across units.
- Individual contact signals are handled via 3-pin connectors, with functions varying by unit (e.g., START OUT for Autosampler).
- Detailed diagrams show connections for L-2000, Chromaster series, and D-2500.
Terminologies (Appendix 3):
Provides definitions for key terms related to the instrument's operation and components, such as e-line, IFC, liquid leak sensor, initialize, warming-up, error message, degassing, log book, binary pump, high-pressure gradient system, injection, loop injection method, Peltier, sample rack, septum, 6-way 2-position valve, column control system, ambient, time program, preheat, gas leak sensor, D2 lamp, Hg lamp, auto zero, grating, output range, slit, instrument parameters, diode array detector (DAD), default, wavelength check, validation, filter, photo diode array, full scale, flow cell, lamp house, sample-side energy, reference-side energy, photo cell circuit board, and half mirror.
Need help?
General
To Next Page