The Primaide 1440 FL Detector is a fluorescence detector specifically designed for the detection of sample components in a liquid chromatograph system. It is intended for use by persons with a basic knowledge of chemical analysis.
Function Description:
The Primaide 1440 FL Detector operates by detecting the fluorescence emitted by sample components. In a liquid chromatograph system, a pump delivers mobile phases, a sample introduction unit (autosampler or manual injector) injects samples, a column separates components, and a column oven maintains the column at a constant temperature. The detector then senses the separated sample components as electric signals. The system can also incorporate a degassing unit for deaerating eluents and a gradient device for varying the mixing ratio of eluents over time.
In an isocratic system, a single solvent analysis is performed. The eluent is fed by the pump through a degassing device, a sample is injected, separated by the column in the column oven, and then detected. In a low-pressure gradient system, multiple eluents are mixed in a low-pressure unit at a pre-specified ratio, delivered through a mixer, and then the sample is injected, separated, and detected.
The detector's front panel includes a power switch, a UI pad (optional keypad for unit operation), and four LED indicators for CH1 (blue for operation, orange for error), CH2 (blue for operation, orange for error), Xe LAMP (blue when lit), and PROG. RUN (blue when time program is in execution). A drain tray is provided for liquid leakage.
The rear panel features an analog signal output unit (optional, providing PROCESSOR, RECORDER, MAKER IN terminals), ground terminals, and a power source connector. The e-line connector transmits acquired signals or spectral data and sends/receives instrument parameter data. It also handles contact signals for START IN (program initiation), ERROR IN (checking errors in other instruments), ERROR OUT (indicating errors in this instrument), and BUSY OUT (indicating operational status). LAMP OFF IN and AUTO ZERO IN are activated by contact signals.
Important Technical Specifications:
- Optical system: Ratio photometry; intensity of transmitted beam is monitored.
- Light source: Xe lamp (150 W) and Hg lamp (for checking wavelength).
- Excitation wavelength range: 200 to 850 nm/Zero order.
- Emission wavelength range: 250 to 900 nm/Zero order. (Photomultiplier must be changed at emission wavelength greater than 731 nm).
- Spectral bandwidth on excitation side: 15 nm.
- Spectral bandwidth on emission side: 15 nm, 30 nm (variable). To separate a spectrum completely, a wavelength interval of 30 nm or more is required.
- Wavelength setting: By communication (e-line) or keyboard.
- Wavelength accuracy: ±3 nm.
- Wavelength repeatability: ±0.5 nm.
- Recorder output (Option): 10 mV Full scale, 1 to 1000 FLU (settable in steps of 1).
- Processor output (Option): 1 V Full scale, digital by e-Line, -40 (-40 mV) to 1000 (1000 mV).
- Response: Changeable in 7 steps corresponding to time constants of 0.05 / 0.1 / 0.5 / 1.0 / 2.0 / 4.0 / 8.0 seconds.
- Sensitivity (S/N ratio for Raman peak of water):
- 15 nm emission-side spectral bandwidth: 700 or more (Baseline method), 525 or more (Tangent method).
- 30 nm emission-side spectral bandwidth: 900 or more (Baseline method).
- Wavelength: 350 nm, Time constant: 2.0 s.
- Auto Zero range: 0 to 1000 FLU.
- Offset range: 0 to 1000 FLU (settable in steps of 1).
- Spectrum memory: Memorizes excitation and fluorescence spectra, up to 4 spectra. Measuring wavelength range is changeable in measurement condition setting.
- Marker (Option): Places a marker (0.6 mV) on the recording.
- Instrumental conditions setup: Full scale range, spectrum measurement range, photo multiplier applied voltage, and offset value are set and saved.
- Time program: Up to 9 programs, 100 steps total. Settable time up to 600 minutes in 0.1 minute increments. Programmable parameters include measurement wavelength (Ex and Em), baseline processing, and PMT gain.
- GLP support function: Lamp energy check, wavelength accuracy check, lamp lighting time, and replacement record.
- Communication facility: e-Line communication.
- External output terminal (Option): Processor (1 V Full scale), Recorder (10 mV Full scale).
- External I/O contact terminals: Time Program Start, Error Input/Output, Busy Output, Auto Zero Input, Lamp Off Input.
- Flow cell: Standard, 12 µL capacity (irradiated capacity), 1.0 MPa withstand pressure.
- Operating temperature range: 4 to 35 °C (non-condensing).
- Operating humidity range: 25 to 85% RH.
- Power requirement: 100-240 VAC/50 or 60 Hz.
- Power consumption: 250 VA.
- Dimensions: 340(W) mm × 464(D) mm × 297(H) mm.
- Weight: Approx. 26.7 kg.
Usage Features:
The UI pad allows for basic operations such as power supply control, parameter setting (wavelength, offset, time constant, PMT voltage, emission bandwidth, error output, leak sensor, lamp ON/OFF), GLP functions (lamp logbook display/resetting, wavelength accuracy check, lamp energy check), time program setting, and spectrum measurement. The UI pad is disabled when a chromato data station is connected.
- Parameter Setting: Values are entered using numeric keys and confirmed with the ENT key. Incorrect operations can be cancelled with the ESC key.
- Auto Zero Adjustment: Resets FL indication and output signal to zero at measuring wavelength.
- Wavelength Setting: Excitation (Ex) and Emission (Em) wavelengths can be set within specified ranges.
- Time Program: Allows automatic changes of measurement parameters over time, including measurement time, excitation/emission wavelengths, baseline processing, and photomultiplier voltage. Up to 9 programs with 100 steps can be registered.
- Spectrum Measurement: Enables measurement and recording of spectral data for excitation and emission scan ranges.
- Marker Operation: Allows placing markers on recordings for event indication.
Maintenance Features:
- Operational Check: Verifies proper setting of measurement conditions, wavelength operation, and auto zero.
- Performance Checks: Includes Xe lamp energy check and wavelength accuracy check using the Hg lamp. The Xe lamp energy level should be checked regularly, and replacement is recommended if it decreases by 50% or more. Wavelength calibration is necessary if accuracy errors exceed ±3 nm.
- Periodic Checks: Daily checks for drain tray, lamp lighting, liquid leakage, and fluorescence intensity. Monthly checks for lamp lifetime and leak sensor. Yearly check for wavelength accuracy.
- Flow Cell Unit Checks: Involves checking and washing the flow cell for contamination or leakage. Disassembly and cleaning procedures are provided.
- Troubleshooting: A comprehensive table lists symptoms, causes, judgment/check methods, and remedies for common issues like excessive drift, poor S/N ratio, poor wavelength accuracy, and leak errors.
- Error Messages: Descriptions and remedies are provided for various error messages, including ROM/RAM errors, parameter errors, wavelength drive mechanism errors, lamp overheating, and data buffer overflow.
- Spare Parts: A list of replacement parts and consumables with estimated service life and remarks is provided to minimize downtime.
- Lamp Replacement: Detailed instructions for replacing both the Xe lamp and Hg lamp, including safety precautions for handling high-pressure lamps and hot parts. Positional adjustment of the Xe lamp is crucial for accurate performance after replacement.
- Fuse Replacement: Instructions for replacing fuses, emphasizing safety precautions against electric shock.
Safety Precautions:
The manual emphasizes reading safety instructions carefully. Warnings are provided for potential hazards such as electric shock, injury from xenon lamp explosion, burns from hot parts, and risks associated with flammable, toxic, corrosive, or stimulative chemicals. Proper grounding, ventilation, and use of protective gear are highlighted. The instrument is not explosion-proof, and certain organic solvents with low ignition points should not be used in unattended operation. Physiologically or biologically active samples are not applicable due to infection risks. Precautions regarding electromagnetic wave disturbance and proper disposal of the instrument and its parts are also included. The instrument bears CE conformity marking for European countries.
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