DSC

Created By: Steve Howard & Mike Shirey

Instruction Manual for Running Differential Scanning Calorimetry (DSC) Test On Powder Coating Materials.
Introduction
This manual provides instructions to prepare a sample and run a DSC test, on powder coating materials, using a Perkin Elmer DSC-6 instrument. DSC tests are used to determine a number of temperature related physical properties such as Tg (glass transition temperature), degree of cure, and reaction onset temperature. The analysis of the DSC results will not be covered in this document. No prior laboratory experience is necessary to accomplish the DSC test. It takes 30 minutes to run the described DSC test.

Sections
Sample Preparation. Loading the DSC. Sample DSC Run. Sample DSC Run Completion

Equipment List
1. Perkin Elmer Sample pans and lids 2. Perkin Elmer Pan Press 3. Tweezers 4. Perkin Elmer DSC 6 Differential Scanning Calorimeter 5. Razor Blades 6. Copy paper (Not shown)

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Indicates a cautionary note. Indicates an instructional note.

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Created By: Steve Howard & Mike Shirey

Step 1 Sample Preparation

Caution: Razor blades are dangerous. Take care to ensure you do not cut yourself during their use. Note: Do not touch the collected sample material, sample pans or lids with your fingers. The DSC test is sensitive to contamination from skin oils and this could affect the accuracy of your results. A. Scrape or cut shavings of the cured powder coating material onto a piece of clean paper, using a razor blade. Collect enough sample material to fill a sample pan. B. Transfer the sample material onto a 3x2 piece of paper with a fold lengthwise down the center as shown.

Step 2 Sample Preparation

Note: Use tweezers to handle sample pans and lids to prevent contamination from hand oils or foreign materials. Note: It is normal for small amounts of the sample to spill as it is transferred into aluminum sample pan. A. Add sample material to the sample pan until it is level with the top edge of the pan. B. Place a pan lid over the sample material in the pan. The lids are non-directional so it does not matter which side is up. C. Press the lid into pan using tweezers.

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Created By: Steve Howard & Mike Shirey

Step 3 Sample Preparation

Note: Use tweezers to handle prepared samples. Note: Perkin Elmer Pan Press [1] with components identified at right: (Labeling was added) A. Using tweezers, place the prepared sample pan on the cylinder body at the base of the pan press. B. Pull the cylinder body downward to expose the center anvil. The cylinder body is spring loaded in the up (closed) position. C. Slide the sample to a centered position over the anvil. D. Gently allow the cylinder body to rise back up into the closed position. E. The sample should now be positioned on top of the anvil, at the bottom of the anvil - cylinder body assembly.

Step 4 Sample Preparation

Note: Use tweezers prepared samples. to handle

A. Push down on the hand pad at the top of the press; this drives a crimping piston into the anvil chamber and seals the pan. Press the pad downward until you hear a soft click, indicating the pan edge has been crimped over the lid. B. Remove the sealed pan from the press by pulling the cylinder body downward to expose the sealed sample pan. Remove with tweezers. C. Place the sealed sample pan on a hard surface, like the press base, and poke a small hole in the top of the pan lid using the tip of the tweezers.

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Created By: Steve Howard & Mike Shirey

The hole allows gasses to escape during the DSC process.

Step 5 Loading the DSC.

Note: Do not remove the sample pan from the cavity on the left hand side of the furnace; this is a calibration standard and must be in place for the test to run correctly. A. Pick up and remove the furnace outer lid, and set it aside. B. Pick up and remove the furnace inner lid, and set it aside. C. Remove the sample pan from the previous DSC run. The sample pan is on the right hand side of the inner furnace. D. Place the sample you just prepared into the recessed cavity on the right hand side of the inner furnace. The pan will center itself on the raised button in the center of the cavity. E. Replace inner furnace access doors. F. Replace outer furnace access door.

Step 6 Sample DSC Run

A. Turn on the computer and the DSC machine. The on-off switch for the DSC machine is at the back of the instrument. B. Wait for the computer to finish its start routine. After startup, the screen will have a number of icons displayed on the left hand side. Double click the Pyris Manager icon.

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Created By: Steve Howard & Mike Shirey

Step 7 Sample DSC Run

Note: When the software is opened, a menu tool bar will appear at the top of the desktop. A. Open the instrument viewer screen by double clicking on the DSC 6 button located on the menu tool bar at the top of the desktop.

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Step 8 Sample DSC Run

Note: The Instrument Viewer screen is a real time graphical display of the instrument. The graph shows endothermic heat flow vs elapsed time. A. Open the Method Editor screen by single clicking on the icon as shown, allowing for user input of the run parameters.

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DSC

Created By: Steve Howard & Mike Shirey

Step 9 Sample DSC Run

Note: The Method Editor screen opens and contains three pages for user entry. These screens are accessed via tabs. A. Click on the sample tab to ensure that it is selected and active. B. Click in the area labeled Sample ID: and enter the sample name; then click in the Operator ID: area and enter operators initials.

Step 10 Sample DSC Run

A. Click on the Initial State tab to activate the Set Initial Values interface. B. Ensure that the Temperature value is set to 40.00C and that the Y Initial value is set to 20.00mW. These are the default values but can be adjusted if necessary by using the arrow buttons next to each entry area.

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Created By: Steve Howard & Mike Shirey

Step 11 Sample DSC Run

A. Click on the Program tab to activate this screen. B. Ensure that the Initial Temp value is set to 30.00C which will be reflected in the highlighted blue area as step 1).

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Step 12 Sample DSC Run

A. Click on the Add a step button located just to the right of the highlighted blue area, step 1). This will open a pop-up window named Method Step Options. B. Select Temperature Scan from list. C. Click on OK button at bottom of pop-up screen to return to program screen.

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Created By: Steve Howard & Mike Shirey

Step 13 Sample DSC Run

A. Ensure that tthe To temperature option is set to 250.00C. B. Ensure that the Rate option is set to 20.00C/min.

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Step 14 Sample DSC Run

A. Click on the End Condition button to enable the End Condition interface area. B. Set the Go To: temperature to 40.00C. Activate the up/down arrows to change the value displayed, or click inside the value display and type the desired value. The end condition value sets the furnace temperature at the completion of the program cycle. C. Click on the Done button.

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Created By: Steve Howard & Mike Shirey

Step 15 Sample DSC Run

A. Press the DSC start/stop run button to begin the program.

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Sample DSC Run Completion

The DSC run will be complete after the equipment reaches the end condition set in Step 14. As stated in the introduction, analysis of the resulting data is beyond the scope of this set of instructions and will be addressed in a separate document. When prompted whether you wish to save the file, click yes. The file will be saved with the sample ID you entered at the start of the test. Differential Scanning Calorimeters work by comparing the ability of two separate samples, placed on two separate heating elements, to take on energy in the form of heat. The DSC measures and graphs the difference in energy needed to maintain both samples at the same temperature, as it runs the programmed heating cycle. The graph is then evaluated for inflection points, peaks and peak areas, to determine results.

[1]

44-70239_02190048TEA3StdSamplePanCrimperPress_220x220 in Perkin Elmer [Online]. Available: http://www.perkinelmer.com/Catalog/Product/ID/02190048