Attachment 1 - Salient Characteristics.pdf

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USAFA - Simultaneous Dynamic Scanning Calorimeter/Thermogravimetric Analyzer (SDT)
Solicitation number
FA700026Q0102
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This document specifies the technical specifications and performance requirements for a Simultaneous Differential Thermal Analysis (SDT) or Simultaneous Thermal Analyzer (STA) instrument.

The SDT/STA must operate across a temperature range from ambient to 1500°C with a 200 mg sample weight capacity. Key technical specifications include weighing precision of ±0.1%, weight sensitivity and resolution of 0.2 µg (2 ppm) or better, weight accuracy of ±0.5% or ±100 µg (whichever is greater), and dynamic baseline drift less than 50 µg across both temperature ranges. The instrument must feature a horizontal null-balance thermobalance design with 0.1 µg sensitivity, a wire-wound furnace capable of vacuum operation at 100 µTorr or better, and integrated dual-gas delivery control with automated switching and programmable flow rates. The DSC sensitivity requirement is 4 µW over 50°C to 1000°C, with heat capacity measurements within ±5% of standard materials, enthalpy accuracy and precision both under 2%, temperature accuracy of ±1°C, and dynamic/isothermal temperature precision of ±0.5°C and ±0.1°C respectively. Linear heating rates must range from 0.1 to 100°C/min in 0.01°C/min increments with forced-air furnace cooling capability from 1500°C to 50°C in less than 40 minutes.

The instrument must include an autosampler accommodating at least 30 samples with mechanical finger-style gripper operation, independent touch-screen control, and capability for unique experiments per sample. Operating software must enable fully automated calibrations (weight, heat flow, heat capacity, cell constant, temperature), automatic periodic software updates via internet connection, unlimited data analysis software installations, and integration with legacy thermal analyzer data (DSC, TGA, TMA, DMA). The instrument requires NRTL certification per OSHA standards with specific documentation provided. Additional requirements include installation, certification, and training; a U.S.-manufactured PC and monitor; a one-year full warranty covering all travel, labor, and parts; five-year extended service protection for furnace failure; Ethernet BUS communication; horizontal purge gas flow capability; easy interface compatibility with Mass Spectrometry or FTIR; and DTA data output in degrees Celsius. The instrument must support multiple heat capacity determination methodologies (single-run direct Cp, ASTM E1269 three-run method, and modulated-temperature methods in conventional, heat-only, and quasi-isothermal modes), automated heating rate adjustment based on decomposition rate, real-time data acquisition viewing, and automatic conversion from heating to isothermal holds based on weight loss parameters.

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Salient Characteristics SDT Analyzer

The SDT or STA should meet or exceed the following technical specifications when evaluated as described for each value:

• Temperature Range: Ambient to 1500 °C

• Sample Weight Capacity: 200 mg

• Dynamic Weighing Range: 200 mg

• Weighing Precision: ± 0.1%

• Dynamic Baseline Drift (50 to 1,000 °C): <50 µg

• Dynamic Baseline Drift (1,000 to 1,500 °C): <50 µg

• Weight Sensitivity: 0.2 µg (2 ppm) or better

• Weight Resolution: 0.2 µg (2 ppm) or better

• Weight Accuracy: ±0.5% of value or ±100µg (whichever is greater)

• Weight Repeatability: ± 0.1% of value or ±50µg (whichever is greater)

• DSC Sensitivity: 4 µW over the temperature range of 50°C – 1000°C

• Heat Capacity Measurements : < +/- 5% of a standard material (e.g. aluminum oxide)

• Enthalpy Accuracy: < 2% (based on metal standards)

• Enthalpy Precision: < 2% (based on metal standards)

• Temperature Accuracy: ±1°C

• Dynamic Temperature Precision: ±0.5°C

• Isothermal Temperature Precision: ±0.1°C

• Linear Heating Rates: 0.1 to 100°C/min in 0.01°C/min increments

• Furnace Cooling: Forced Air 1500°C to 50°C in < 40 min

Instrument Features

Thermobalance

The SDT or STA must employ a horizontal null-balance design. True balance sensitivity of 0.1 µg or better is required.

Furnace

The furnace is a wire-wound furnace. The combined thermobalance and furnace is capable of operating in vacuum of 100 µTorr or better.

Gas Delivery

The SDT or STA must include integrated purge gas delivery control accommodating two simultaneously installed gases. This capability must be incorporated into the instrument (i.e.

shall not be a separate unit). Purge gas flow rate must be programmable within operating software, and deliverable as a saved signal in the data file. Gas delivery control must also allow for automated switching between the gases during an experiment. An optional accessory will allow blending of binary mixtures of gases in controllable ratios. The SDT or STA should include a horizontal gas purge system to provide highly accurate and precise control purge gas flow rate and gas switching capability. The system software should include automatic buoyancy corrections for temperature and gas flow rate.

Autosampler Performance

The SDT or STA should include an autosampler that can be configured to accommodate at least

30 samples and allow for unattended operation and data acquisition. The reference pans should be configurable to any of the positions in the autosampler tray. The autosampler shall employ mechanical finger-style gripper, not a suction device. The autosampler shall be controllable through a touch-screen display, or by some other means independent of the controlling computer. The autosampler shall not require regular lubrication. Software shall include auto-tare feature to tare each pan unattended. Instrument must be capable of performing a unique experiment on each sample within one loaded sample tray. The SDT or STA shall employ position calibration routines via a touch screen to ensure reliable performance.

Software

The SDT or STA must include operating software which allows for the instrument to be fully calibrated and verified automatically. Calibrations must include weight, heat flow, heat capacity, cell constant and temperature. The operating software should also be capable of periodically and automatically checking for updates via an internet connection, and downloading/installing those updates if desired. The data analysis software should allow for unlimited installations. The data file format should easily allow sharing/transfer of data files as individual electronic documents, which are readable by the same data analysis package. The data analysis program should also include a .pdf generator, for the efficient export of analyzed plots. Software updates

(for either “bug fixes” or subsequent enhancements) must be provided for the lifetime of the SDT or STA instrument. The supporting software must have the ability to perform all calibrations

(verification, re-calibration if needed, re-verification if re-calibrated) in a completely unattended manner during quiescent times (e.g., Sunday morning at 0600). The software must offer the ability to integrate (overlay, analyze, etc.) legacy data from our existing thermal analyzers (DSC, TGA, TMA, DMA).

NRTL Certification:

As required by OSHA product safety standards, the instrument must be NRTL certified, and carry the certification mark of the specific NRTL laboratory. Products that bear only non-NRTL certification marks (including the CE mark) do not meet the OSHA standard requiring NRTL approval of the product. In addition, specific documentation regarding NRTL certification must be provided with the proposal/bid package.

Additional Features and Requirements

Installation, certification, and training should be included.

A PC and monitor must be included.

The PC and monitor must be made in the United States.

Full one-year warranty covering all travel, labor and parts required for SDT or STA to meet specifications.

Extended service protection that covers the cost to replace furnace failure for a period of five years after installation.

The SDT or STA must be easily interfaced to a Mass Spectrometer or FTIR, with either option being able to add later.

The SDT or STA must employ horizontal purge gas flow to minimize buoyancy effects from purge gas and for direct output to off gas analysis.

The SDT or STA should have a reactive gas inlet that allows for reactive gases to be introduced to the sample without contamination of the balance.

The SDT or STA shall include DTA data in degrees Celsius.

The SDT or STA must include touch screen capable of recalling and running preprogrammed methods, loading, taring, and monitoring running experiment.

The SDT or STA must communicate with computer/controller through Ethernet BUS.

Data files contain measured sample temperature, not calculated temperature.

The SDT or STA must demonstrate the ability to continuously measure sample weight loss of up to 200 mg.

The SDT or STA must employ push button automatic loading and unloading of sample pan.

Operator does not have to place the pan on the beam in normal use.

The SDT or STA must demonstrate ability to have up to five points for temperature calibration to provide greater temperature accuracy over wide temperature ranges. It must be capable of melting point calibrations as well as Curie Point temperatures with an external magnet.

Ability to abort a test and/or segment in a test when operator specified conditions are met.

The SDT or STA must have local control at the module including experiment start/stop and real-time display of sample temperature and experiment status.

The SDT or STA must have automatic recording of initial sample weight.

The SDT or STA must have the ability to continue a run when disconnected from the computer/controller.

The SDT or STA must have the ability to store calibration constants in module memory.

Heat capacity measurements must not require a prior baseline scan that has to be subtracted from the sample scan for quantitative data.

The SDT or STA must provide heat capacity determination by all of the following methodologies:

• Single run (direct Cp) method

• ASTM E1269 three-run (baseline, calibrant, and sample) method

• Modulated-temperature methods:

o Conventional mode (allows sample heating and cooling during temp ramp) o Heat-only mode (allows only sample heating during temp ramp) o Quasi-isothermal mode (Cp determination isothermally at specified temperatures)

The SDT or STA must be capable of automatically and continuously changing the heating rate as a function of decomposition (sample weight loss).

The SDT or STA must be capable of automatically changing from heating to an isothermal hold when pre-selected limits of weight loss in %/min is met.

The SDT or STA must be capable of automatically and continuously changing the heating rate to achieve a pre-determined rate of sample decomposition expressed in %/min.

Must be able to view data acquisition and signals in real time.

Instrument Features
Thermobalance
Additional Features and Requirements

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