Selecting a Sample Pan

Selection of the appropriate DSC sample pan and lid is a very important element of your method development process. The results you obtain from the use of DSC will be affected by your choices. The subject of methods development is covered in depth during the various training courses available from TA Instruments.

TA Instruments offers various types of DSC pans for use in your experiments. Use the following guidelines to select a sample pan material and configuration that meets the temperature and pressure range, composition, and reactivity requirements of your experiment.

Click on the follow topics for more information:

• Selecting a Sample Pan for the Tzero Press

• Tzero Series Pans

• Standard Series Aluminum Pans

• Pan Types

• Additional Tzero Pan Information

• Selecting a Pan for the Beige or Blue_Press

• Crimped and Hermetic Sample Pans

• High Volume and High Pressure Pans

• Pan Resistance Correction (used for Tzero measurements only)

• Preparing DSC Samples

Selecting a Sample Pan for the Tzero Press

There are two series of DSC pans available for use with the Tzero Press. The Tzero Series sample pans and lids are manufactured using a sophisticated manufacturing process to higher design specifications and their use typically results in improved resolution, sensitivity and enthalpy repeatability compared to the Standard Series sample pans and lids. The Standard Series is suitable for general-purpose use and provide a balance between performance and cost.

Within each series, the following pan types are currently available. Factors to consider when choosing a pan type are described briefly below.

Tzero Series Pans

• Tzero Aluminum

• Tzero Low-Mass Aluminum

• Tzero Aluminum Hermetic

• Tzero aluminum Hermetic Alodined

Standard Series Aluminum Pans

• Standard Aluminum

• Standard Aluminum Hermetic Alodined

Pan Types

There are three types of Tzero pans available, the Tzero Pan (901683.901), Tzero Alodined Pan and the Tzero Low-Mass Pan (901670.901).

There are also three types of lids available, the Tzero Lid (901671.901), Tzero Hermetic Lid (901684.901), and Tzero Hermetic Alodined Lid.

These pans and lids are used to make three main pan types, which are described below:  Tzero Aluminum, Tzero Hermetic Aluminum, and Tzero Low-Mass Aluminum. (For more detailed information on the various pan configurations, click here  Additional Tzero Pan Information).

• The Tzero Aluminum Pan is formed from the combination of the Tzero Pan and the Tzero Lid.  It is used for most DSC applications where there is not a need for hermetic sealing.  This pan type has a large capacity in volume (ca. 21 mL) and mass.  These pans are formed using the black die set for the Tzero press.  Choose “Tzero Aluminum” as the pan type in the Advantage software when using this pan.

• The Tzero Hermetic Aluminum Pan is formed from the combination of the Tzero Pan and the Tzero Hermetic Aluminum Lid.  This is a high-volume pan (ca. 40 mL) and is ideal when hermetic sealing is required, or when volatiles need to be contained.  This pan type is sealed using the blue die set for the Tzero press.  Choose “Tzero Hermetic Aluminum” as the pan type in the Advantage software when using this pan.  

• For samples which contain large amounts of evolved water, it may be preferable to use the Tzero Hermetic Aluminum Alodined Pan. At higher temperatures and pressure, water can react with the aluminum used to make these pans. This exothermic reaction can in some cases interfere with your measurement. An inorganic alodine treatment applied to the Tzero aluminum hermetic pans eliminates the interference caused by the water in the sample. This pan type is sealed using the blue die set for the Tzero press.  Choose “Tzero Hermetic Aluminum Alodined” as the pan type in the Advantage software when using this pan.  

• The Tzero Low-Mass Aluminum Pan is formed from the combination of the Tzero Low-Mass Pan and the Tzero lid.  This is a specialty pan type, which is ideal for high-sensitivity applications on small amounts of material (<10 mg).  This pan type is sealed using the black die set for the Tzero press.  Choose “Tzero Aluminum” as the pan type in the Advantage software when using this pan. (NOTE: Tzero Hermetic Lids should not be used with Tzero Low-Mass Pans).

The various pan type configurations are summarized in the following table:

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Additional Tzero Pan Information

Tzero Aluminum Pan (Tzero Pan and Tzero Lid)

• 901683.901 Tzero Pans (Pkg/100)

• 901671.901 Tzero Aluminum Lids (Pkg/100)

The Tzero Aluminum Pan is an excellent choice for the majority of applications where volatiles are not an issue. The performance of the Tzero pan is exceptional due to the precise flatness of the pan bottom and the contact of the lid to the upper surface of the sample.

The Tzero Pan and Tzero Lid packages are labeled with a black/blue stripe and a solid black stripe, respectively. The Tzero Press includes three dies with a black ring that are easily recognized and are used with these pans and lids. The lower die is readily distinguished from the upper dies by a larger outer diameter compared to the upper dies. See also: Encapsulating a DSC Sample with the Tzero Press

The design of the Tzero Lid and Tzero Press helps ensure that the pan bottom remains flat after sample loading. The lower die has a flat surface to support the pan bottom and minimize deformation from the sample when pressing the lid in place. You may choose either of two upper dies—one is flat and the other concave. The flat die is typically the first choice so that the sample-to-pan and sample-to-lid contact can be maximized. However, use of the concave die may be advantageous for irregularly shaped samples, as the lid will tend to conform to the sample better.

When using the Tzero Aluminum Pan, the maximum volume is 20 µL. The maximum height of the sample should be 1.0 mm (0.039 in) or less in order for the lid to properly engage the pan. The average mass of the pan and lid is about 49.7 mg with a typical variability of 0.75%. Advanced Tzero support available with the Q2000 minimizes the impact of the higher mass, while the superior flatness of the pan bottom improves the sensitivity, resolution and enthalpy repeatability of the heat flow measurement to levels never before achieved in routine practice.

The Tzero Pans and Lids are made of high purity aluminum and do not contain any intentional alloying elements. They are formed into their precisely designed shapes by an impact extrusion process that uses high pressure and a series of progressive dies to flow the aluminum into the precise shape of the tooling. Reliable adherence to stringent design specifications is achieved using this process. The Tzero Press and Pans represent the new state of the art in DSC sample preparation tools.

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Tzero Hermetic Aluminum Pan (Tzero Pan and Tzero Hermetic Lid)

• 901683.901 Tzero Pans (Pkg/100)

• 901684.901 Tzero Hermetic Lids (Pkg/100)

The Tzero Hermetic Aluminum Pan is exceptional for applications whenever volatiles generated by the sample during the experiment interfere with the transitions of interest.

The performance of the Tzero Hermetic Aluminum Pan is outstanding due to the precise flatness of the pan bottom and the design of the upper lid and sealing mechanism.

The Tzero Pan and Tzero Hermetic Lid packages are labeled with a black/blue stripe and a solid blue stripe, respectively. The Tzero Press kit contains a set of two dies with a blue ring that used with these pans and lids. The lower die is easily distinguished from the upper die by a larger outer diameter. See also: Encapsulating a DSC Sample with the Tzero Press

The Tzero Hermetic Lid is readily sealed to the Tzero Pan by a cold welding process that uses pressure applied by the upper die in the Tzero Press to join the two aluminum surfaces together. The sealing process does not exert any force on the bottom of the pan and the pan bottom remains flat. The pressure seal formed will typically hold 2-3 atmospheres of internal pressure. When pressurized above 2 atmospheres, the lid will deform outward, with the bottom of the Tzero Pan in contact with the DSC sensor remaining flat.

When using the Tzero Hermetic Aluminum Pan the maximum volume is 40 µL. The maximum height of the sample should be less than 1.9 mm (0.075 in) in order for the lid to properly sit on the sealing surface of the pan. The average mass of the pan and lid is 50.5 mg with a typical variability of 0.75 %. Advanced Tzero support available with the Q2000 minimizes the impact of the higher mass, while the superior flatness of the pan bottom improves the sensitivity, resolution and enthalpy repeatability of the heat flow measurement to levels never before achieved in routine practice.

The Tzero Pans and Tzero Hermetic Lids are made of high purity aluminum and do not contain any intentional alloying elements. They are formed into their precisely designed shapes by an impact extrusion process that uses high pressure and a series of progressive dies to flow the aluminum into the precise shape of the tooling. Reliable adherence to stringent design specifications is achieved using this process. The Tzero Press and Pans represent the new state of the art in DSC sample preparation tools.

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Tzero Low-Mass Aluminum Pan (Tzero Low-Mass Pan and Tzero Lid)

• 901670.901 Tzero Low-Mass Pans (Pkg/100)

• 901671.901 Tzero Lids (Pkg/100)

The Tzero Low-Mass Aluminum Pan is intended for small size samples that may benefit from the lower mass of the pan. The performance of the Tzero Low Mass pan is exceptional due to the precise flatness of the pan bottom and the contact of the lid to the upper surface of the sample.

The Tzero Low-Mass Pan and Tzero Lid packages are labeled with solid black stripes. The Tzero Press includes three dies with a black ring that are easily recognized and are used with these pans and lids. The lower die is readily distinguished from the upper dies by a larger outer diameter compared to the upper dies. See also: Encapsulating a DSC Sample with the Tzero Press

The design of the Tzero Low Mass Lid and Tzero Press helps ensure that the pan bottom remains flat after sample loading. The lower die has a flat surface to support the pan bottom and minimize deformation from the sample when pressing the lid in place. The user may choose either of two upper dies; one is flat and the other concave. The flat die is typically the first choice so that the sample to pan and sample to lid contact can be maximized. However, use of the concave die may be advantageous for irregularly shaped samples, as the lid will tend to conform to the sample better.

The maximum volume of the Tzero Low-Mass Pan is 10 µL. The maximum height of the sample should be 0.51 mm (0.020 inches) or less in order for the lid to properly engage the pan. The average mass of the pan and lid is about 28.4 mg with a typical variability of 0.60%. Advanced Tzero support available with the Q2000 and the superior flatness of the pan bottom improves the sensitivity, resolution and enthalpy repeatability of the heat flow measurement.

The Tzero Pans and Lids are made of high purity aluminum and do not contain any intentional alloying elements. They are formed into their precisely designed shapes by an impact extrusion process that uses high pressure and a series of progressive dies to flow the aluminum into the precise shape of the tooling. Reliable adherence to stringent design specifications is achieved using this process. The Tzero Press and Pans represent the new state of the art in DSC sample preparation tools.

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Selecting a Pan for the Beige or Blue Press

TA Instruments offers various types of DSC pans for use in your experiments. Use the following guidelines to select a sample pan material and configuration that meets the temperature and pressure range, composition, and reactivity requirements of your experiment.

The three types of pans within the Standard Series serve similar purposes. The main factor to consider when choosing one of these three pan types is whether the sample contains or will evolve volatiles and/or water.

• The Standard Aluminum pans are the common first choice. These pans use lids that are pressed down into contact with the sample and essentially encapsulate the sample in aluminum and thereby maximize the quality of the heat flow measurement. However, these types of lids are not sealed to prevent the loss of volatiles present in or generated by the sample during the experiment. Often, if these volatiles are allowed to evaporate, the endothermic heat flow associated with the vaporization obscures the transitions of interest. In some cases, the sample itself can flow out of these pans at higher temperatures and contaminate the cell.

• The Standard Aluminum Hermetic pans have a different type of lid and sealing mechanism that is able to hold the pressure buildup due to these volatiles. This pressure can reach up to 2-3 atmospheres before the sealed pan releases the pressure. In many applications, the buildup and retention of the self-generated atmosphere by the sample improves the resolution of the transitions of interest.

• The third type of pan, the Standard Aluminum Hermetic Alodined pans, are used when samples have high water content. At higher temperatures and pressure, water can react with the aluminum used to make these pans. This exothermic reaction can in some cases interfere with your measurement. An inorganic alodine treatment applied to the aluminum hermetic pans eliminates the interference caused by the water in the sample.

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Crimped and Hermetic Sample Pans

In an ideal DSC experiment, the sample material would be placed directly on the DSC sensor to obtain optimum heat transfer. However, that is not practical due to potential contamination of the sensor. Therefore, samples are placed in sample pans for analysis. The table below shows the common types of crimped and hermetic sample pans and their recommended temperature ranges.

NOTE:  The useable temperature range could be reduced by the cooling accessory being used.

Indicates pans designed for use with the DSC Autosampler.

Indicates pans designed for use with the DSC Autosampler and requires the Autosampler Sample Pan Tray PN 971126.90.

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Additional Information About Crimped Pans

• Standard Series pans are designed to be run either open (no lid) or with a lid (crimped) on top of the sample. The lid is usually used to flatten the sample against the bottom of the pan for improved thermal contact. In both configurations crimped pans provide the opportunity for good sample–atmosphere (purge gas) interaction.

• Crimped pans are available in aluminum, gold, copper, platinum, and graphite. (NOTE:  The platinum and graphite pans have no lids.)

• Aluminum pans are used for most experiments unless temperatures above 600°C are of interest for your sample or the sample reacts with aluminum.

• Copper pans are widely used for oxidative stability experiments, particularly for polymeric materials used as wire and cable coatings.

• Graphite pans are used for evaluating materials that might alloy with the various metal pans. Graphite pans should be used with a non-oxidizing purge gas (such as nitrogen).

• SFI (Solid Fat Index) pans are designed specifically for evaluating edible fats and oils. They have a recessed rim around the bottom of the pan to prevent "wicking" due to surface tension.

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Additional Information About Hermetic Pans

• Hermetic pans are designed for evaluation of materials under self-generated atmosphere and/or modest pressure. Hermetic pans are almost always run sealed and are valuable for studies of volatile liquids (including vapor pressure studies), materials that sublime, and materials that generate corrosive or condensable gases.

• Aluminum hermetic pans (sealable to 3 atm. of internal pressure) are used for most samples. Alodined aluminum pans are used to evaluate samples that react with "untreated" aluminum (e.g.,, aqueous biological materials).

• A modified lid, which contains a pinhole of specific known diameter, is available for vapor pressure studies in the aluminum hermetic pans.

• Gold hermetic pans are designed for evaluating materials under higher, self-generated pressures (up to 6 atm.) and temperatures (up to 725°C).

• Hermetic pans, however, do provide a poorer thermal contact between the sample, pan and disk. This fact, plus the added mass of the hermetic pans and covers, leads to a slight loss of resolution compared to the crimped pans.  The calorimetric accuracy is not affected, only the time constant of the system and the resolution of the measurement.

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High Volume and High Pressure Pans

These pans are "specialty" pans designed for specific applications. the table below shows the temperature and pressure ranges appropriate for each type of pan.

Indicates pans designed for use with the DSC Autosampler.

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Additional Information About the Specialty Pans

• High volume pans are stainless steel, disposable pans designed for evaluating liquid samples up to 75 µL. They are particularly useful for measuring weak transitions in aqueous-based biological and food samples. The pans can be sealed to withstand modest pressures so that these materials can be evaluated under self-generated atmospheres. Although the material of construction (stainless steel) will withstand exposure to temperatures above 250°C, it is not recommended that these pans be used above this temperature because rupture of the pan at that point could damage the DSC cell.

To open a printable manual containing  more information regarding high volume pans, click following link:

DSC High Volume Pan Manual

• High pressure capsules are stainless steel capsules sealable to withstand up to 1450 psi internal pressure. They are specifically designed for pressure studies (evaluation of materials under self-generated atmospheres) and have a gold-plated copper rupture disk, which releases pressure gradually when it fails so that no DSC cell damage occurs. High pressure capsules can be reused.

To open a printable manual containing  more information regarding high pressure capsules, click the following link:

DSC High Pressure Capsule Manual

NOTE:  The DSC Autosampler can be used with the high volume pans, but not with the high pressure pans. Click on the link above for more information.

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Pan Resistance Correction (Q2000/Q1000 Only)

The DSC Q2000/Q1000 provides a more accurate measurement of true sample heat flow by accounting for heat flow within the DSC cell sensor as well as between the sensor and the sample pan. The resultant sample heat flow is designated as T4P heat flow.

The heat flow between the sensor and sample pan is primarily affected by the sample pan thermal resistance, which, in turn, is a function of the pan material (thermal conductivity) and temperature, assuming that both the pan and sensor are perfectly flat surfaces and in intimate contact. This assumption, however, is not true, even if careful experimental procedure is followed when preparing samples. Therefore, the thermal resistance of the thin layer of purge gas between the pan and sensor must also be considered.

TA Instruments has included in the Q Series™ Thermal Advantage software fixed values for both pan and purge gas thermal resistances. Available pan choices include aluminum, hermetic aluminum, hermetic aluminum alodined, gold, hermetic gold, large volume, and "other." Purge gas choices include air, nitrogen, oxygen, helium, and outside purge.  When running experiments in Advanced Tzero mode, select the pan type and purge gas that will be used. If you are using a pan type and/or purge gas that is not among the available choices listed, select "other."

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