N0016725Q0044 Minimum Specifications.pdf

MINIMUM REQUIREMENTS – DISCOVERY TGA 5500

1.0 MINIMUM REQUIREMENTS

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

Sample Weight Capacity: 1000 mg

Defined as the maximum sample weight measurable (independent of pans)

Dynamic Weighing Range: 1000 mg

Defined as the maximum measurable weight change (independent of pans)

Weighing Precision: ± 0.01%

Defined as the standard deviation of at least 10 measurements of a 100 mg standard weight, with removing and replacing the sample in between each measurement

Dynamic Baseline Drift (50 to 1,000 °C): <10 µg, with platinum pans

Defined as the maximum deviation from the smallest measured weight to the largest measured weight of an empty platinum pan, while being heated at 20 °C/min in flowing nitrogen atmosphere (without any blank subtraction applied) or any post-test scheme applied

Baseline Linearity (50 to 1,000 °C): <1 µg, with platinum pans

Defined as the average absolute deviation from a best fit linear regression of a baseline scan without any smoothing or blank subtraction applied

Signal Resolution: 0.002 g

Defined as the smallest measurable difference between two adjacent values

Sensitivity: < 0.1 g (1 ppm)

Defined as 3X the average rms noise over the temperature range 50 to 1,000 °C

Temperature Range: ambient to 1200 °C

Defined as the measured temperature at the sample thermocouple (not furnace temperature or programmed temperature)

Temperature Accuracy: ±1 °C

Defined as the standard deviation of the measured error (at least 10 replicate runs after temperature calibration) of the onset temperature of a nickel Curie Point measured at 10 °C/min, removing and replacing the sample in between each run

Dynamic Temperature Precision: ±1 °C

Defined as the standard deviation of the measured Curie Point temperature of at least 10 nickel runs, removing and replacing the sample in between each run

Isothermal Temperature Precision: ±0.1 °C

OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE:

Linear Heating Rates: 0.1 to 500 °C/min in 0.01 °C/min increments

Ballistic Heating Rates: > 1500 °C/min

Furnace Cooling: Forced Air 1000 °C to 35 °C in < 10 min.

2.1 Instrument Design

ThermoBalance Design: Symmetric Vertical Hang-down (Tru-Mass) Furnace type: Infrared heating with built in electromagnetic coil for automated temperature calibration Gas Delivery Manifold: 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.

Autosampler: 25 sample carousel with automated pan punching

2.2 Instrument Features

The TGA shall include high-sensitivity thermobalance, as described below.

The TGA shall include IR-radiation furnace, as described below.

A reactive gas inlet allows for reactive gases to be introduced to the sample without contamination of the balance.

The unit can be configured to provide DTA data in degrees Celsius.

The TGA shall include Hi-Res TGA as described below.

The TGA must be easily interfaced to a Mass Spectrometer or FTIR and shall accommodate a heated purge gas outlet to minimize condensation. The relative temperature of the heated outlet must be software controlled.

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

The TGA must communicate with computer/controller through Ethernet BUS.

Data files contain measured sample temperature, not calculated temperature. This allows the user to know what temperature the sample is at during different heating rate experiments and makes for accurate and precise transition temperatures.

The TGA must demonstrate the ability to continuously measure sample weight loss of up to 1 g.

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

The TGA must employ push button automatic loading and unloading of sample pan. Operator does not have to hang pan on wire in normal use.

The TGA 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 temperature calibration using an integrated electromagnet, the power of which can be preset.

2.3 OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE: Thermobalance (Tru Mass)

The TGA must employ a vertical null-balance design for accurate, precise, and reliable weighing of samples. It must be well insulated, electrically grounded, separately gas purged, and thermally isolated from the furnace. This is essential for high performance baseline performance.

2.4: OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE: Furnace

The furnace should employ infrared heating with a ceramic IR absorber for the rapid response needed for the most demanding applications in standard and high heating rate operation. Furnaces employing metal heater windings are not acceptable. It should also have an internal quartz liner to permit direct operation as an Evolved Gas Analysis (EGA) furnace to handle decomposition products that might adhere to furnace internal features.

The furnace design should include a horizontal gas purge system using Gas Delivery Module 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.

The furnace must include integrated electromagnetic coil for convenient Curie Point temperature calibration of the instrument. The coil power is software controlled.

The combined thermobalance and furnace can operate in vacuum of 50 µTorr.

2.4 Software: TRIOS

The TGA must include operating software which allows for the instrument to be fully calibrated and verified automatically, without the need for operator presence. Calibrations must include weight 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 be unkeyed, to allow for unlimited installations within one site.

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.

2.5 Autosampler Performance

The TGA must include an autosampler that will hold up to twenty-five samples. The method of sample loading / unloading must not disturb the balance.

Tray shall be removable to expedite sample loading and unloading.

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.

OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE: The autosampler must be capable directly punching sealed pans under force control and in a contamination-free manner.

Direct piercing by a sharp “awl- like” mechanism does not constitute a contamination–free process. The system must have the capability of rejecting any pan that is not pierced. This is to prevent a sealed pan being loaded into the TGA furnace.

The TGA shall employ position calibration routines via the touch screen to ensure reliable performance. Total calibration of position shall take no more than 5 minutes.

2.5 OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE: High Resolution TGA (Hi-Res TGA)

Hi-Res TGA is defined as an advanced heater control technology to optimize weight loss resolution using the following (3) modes. All modes are used to separate overlapping transitions.

1) Dynamic Heating Rate to change heating rate automatically and continuously as a function of decomposition (sample weight loss).

2) Constant Reaction Rate to automatically and continuously change heating rate to achieve a pre-determined rate of sample decomposition expressed in %/min.

3) Stepwise Isothermal to automatically change from heating to an isothermal hold when pre-selected limits of weight loss in %/min are met.

2.6 OPTIONAL WITH THE ABILITY TO UPGRADE AT A LATER DATE: Modulated

TGA

Modulated TGA is defined as:

• The ability to apply sinusoidal temperature wave to a sample. Amplitude of sine wave ± 0.01 to 10 °C; period from 100 to 1000 seconds.

• Calculates and displays the following kinetic parameters of decomposition on a continuous basis in real time, Activation energy (kJ/mol) Log (Pre-exponential factor) (1/min) ln (rate ratio)Weight amplitude (mg/min) Modulated Temp (°C)

• Delivers the above kinetic parameters of decomposition in a single scan (data file);

no need for multiple scans.

• Kinetic parameters calculated using a Discrete Fourier Transformation.

• Can modulate temperature during quasi-isothermal methods to evaluate the decomposition kinetics of a single weight loss.

•Can be used with the Hi-Res (variable heating rate) temperature programs to reduce test time.

2.7 Various Features

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

Vertical balance design with automated furnace closing and experiment initiation in one keystroke.

Must have local control at the module including experiment start/stop and real-time display of sample temperature and experiment status.

Automatic recording of initial sample weight.

Automated push button taring. One button push loads pan, raises furnace, tares pan, and unloads pan.

Ability to continue a run when disconnected from the computer/controller.

Ability to use pans up to 250 ul volume to fit larger samples on the thermobalance.

Ability to store calibration constants in module memory.