Physical Address
304 North Cardinal St.
Dorchester Center, MA 02124
D3417-99 – Standard Test Method Technical Guide
📋 Scope and Specimen Types
This test method covers the determination of heat of fusion and heat of crystallization of polymers by differential scanning calorimetry (DSC). It is applicable to polymers in granular form (below 60 mesh preferred, avoid grinding if possible) or to any fabricated shape from which appropriate specimens can be cut.
The normal operating temperature range is from the cryogenic region to 600°C. Values in SI units are to be regarded as the standard.
| 🟦 Parameter | 📏 Specification | 📐 Notes |
|---|---|---|
| Temperature Range | Cryogenic to 600°C | Accuracy may be affected above 400°C due to radiation losses |
| Specimen Form | Granular (below 60 mesh preferred) or cut shapes | Avoid grinding if possible |
⚙️ Test Procedure and Calibration
This test method consists of heating or cooling the test material at a controlled rate in a specified purge gas at a controlled flow rate. The areas under the crystallization exotherm or fusion endotherm are compared against similarly treated areas from a well-characterized standard.
Calibration of heat flow must follow Practice E 968. The method may be combined with Test Methods D 3418 or E 794 for simultaneous melting and crystallization temperature determination.
| 🟦 Reference Standard | 📐 Description |
|---|---|
| ASTM E 968 | Practice for Heat Flow Calibration of DSC |
| ASTM E 793 | Test Method for Heats of Fusion and Crystallization by DSC |
| ISO 11357-1/3 | Plastics DSC – General Principles and Enthalpy Determination |
📊 Key Measured Properties
The test method provides a rapid determination of enthalpy changes for first‑order transitions. It measures heat of fusion, heat of crystallization, and annealing effects in polymers that exhibit these transitions.
DSC can assist in identifying specific polymers, polymer alloys, and additives with thermal transitions. True heats of fusion require additional structure investigation and often specialized crystallization techniques.
⚠️ Warning: Uncertain radiation losses at temperatures higher than 400°C may affect the accuracy of results.
💡 Tip: Use with Test Method D 3418 or E 794 to simultaneously determine melting and crystallization temperatures.
❓ Frequently Asked Questions
🔍 What is the applicable temperature range for this test method?
The normal operating temperature range is from the cryogenic region to 600°C.
💡 What specimen forms are acceptable?
Polymers in granular form (below 60 mesh preferred) or any fabricated shape from which appropriate specimens can be cut. Avoid grinding if possible.
⚡ What factors can affect the accuracy of results?
Uncertain radiation losses at temperatures higher than 400°C may affect accuracy. True heats of fusion require structure investigation and specialized crystallization techniques.
📌 Is this test method equivalent to ISO standards?
It is similar but not equivalent to ISO 11357‑1 and 11357‑3. The ISO standard provides additional information not supplied by this test method.