GB/T 47879-2026Plastics - Fast differential scanning calorimetry (FSC) - Chip calorimetry (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents".

Drafting.

This document is modified to adopt ISO 23976:2021 "Fast Differential Scanning Calorimetry (FSC) for Plastics - Chip Calorimetry".

Compared with ISO 23976:2021, this document has undergone the following structural adjustments.

---3.2 corresponds to 3.6 in ISO 23976:2021;

---Chapter 4 contains content corresponding to section 3.2 of ISO 23976:2021;

--- Section 5.1 corresponds to section 3.1 in ISO 23976:2021.

The technical differences between this document and ISO 23976:2021, and the reasons therefor, are as follows.

a) ISO 11357-1 (see Chapters 1, 3, 5.4, 5.5, 8.2 and 13) has been replaced by the normatively referenced GB/T 19466.1.

(Chapter), to adapt to my country's technological conditions and increase operability;

b) The terms "chip sensor," "chip calorimetry," "sample," and "test specimen" have been removed, and specifications have been added to the introductory texts for terms and definitions.

The referenced standard GB/T 2035 (see Chapter 3) is used to adapt to my country's technical conditions and increase operability;

c) The requirements for specimen quality have been changed (see Chapter 4) to better suit actual test conditions and increase operability;

d) Requirements for sample quality have been added (see Chapter 6), emphasizing the range of sample quality selection to facilitate the application of this document;

e) An explanation of Figure 5 has been added (see 8.2.3), emphasizing the importance of sampling quality requirements and facilitating the application of this document;

f) Added "Calibrate according to the method specified in GB/T 19466.1" (see 8.4), providing a specific calibration reference document and adding steps.

The completeness of the steps facilitates the application of this document;

g) Change "Process the recorded data according to the thermal effects obtained from the instrument manufacturer's instructions and relevant materials" to "According to..." the GB/T 19466 series of standards specifies the processing of recorded data. (See 9.3.4), providing specific data processing reference documents and adding...

Operability, facilitating the application of this document;

h) ISO 11357-3 (see 10.2, 12.4) has been replaced with the normatively referenced GB/T 19466.3 to adapt to my country's technical requirements.

Add components to increase operability;

i) ISO 11357-5 (see 10.3) has been replaced with the normatively referenced GB/T 19466.5 to adapt to my country's technical conditions, and additional...

j) ISO 11357-2 (see 10.4, 12.3) has been replaced with the normatively referenced GB/T 19466.2 to adapt to my country's technical requirements.

Add components to increase operability;

k) ISO 11357-4 (see 12.2) has been replaced with the normatively referenced GB/T 19466.4 to adapt to my country's technical conditions, and additional...

Operability;

l) Change "Test Date" to "Test Personnel and Date" (see Chapter 14) to increase operability.

The following editorial changes have been made to this document.

a) The text "Information on thickness, temperature gradient and scan rate" is changed to Note 1, Note 2 and Note 3 (see Chapter 1);

b) The scope description has been refined (see Chapter 1);

c) Notes 1 and 2 have been deleted (see Chapter 1 of ISO 23976:2021);

d) Change "Sensor heat capacity is independent of sample" to note (see 3.2);

e) The description of the principle is more detailed (see Chapter 4);

f) The equipment name in this document shall be uniformly referred to as "Fast Differential Scanning Calorimetry (FSC) Instrument" (see 5.1, 8.2.2, 8.2.3, 8.2.4, 8.3.2, and Chapter 13);

g) The information regarding environmental conditions for equipment placement has been changed to Note 1 and Note 2 (see 7.1);

h) The information on the three liquid crystal materials reported in the literature for checking the temperature symmetry of rapid scanning calorimeters is changed to note (see 8.3.1);

i) Added "Note. This operation may damage the chip sensor." (See 9.2);

j) Change "Use FSC reference specimen" to "Estimate specimen mass based on known FSC specimen mass" (see 12.6);

k) The description of the precision data has been summarized, and the "Information on Precision" has been changed to a note (see Chapter 13).

Please note that some content in this document may involve patents. The issuing organization of this document assumes no responsibility for identifying patents.

This document was proposed by the China Petroleum and Chemical Industry Federation.

Introduction

This method measures the thermal properties of minute samples (such as thin films and bulk materials) at ultra-high speeds (104 K/s). This type of quasi-adiabatic thermodynamic method can only be used for heating molds.

This method, by introducing gas as a thermally inert coolant, further extends the sensor technology to rapid cooling processes under non-adiabatic conditions.

A smaller sample mass can effectively avoid significant thermal hysteresis caused by increased scanning rate. Therefore, reducing the sample and heating element to a very small size is crucial.

The scanning rate working window of the orimetry (DSC) instrument has been expanded to more than 7 orders of magnitude.

Various studies have shown that the advancements in this technology are based on the ultrafast speeds of micro-electro-mechanical systems (MEMS).

The development of chip calorimeters. Table 1 lists their typical characteristics. Currently, many universities have used specific equipment to obtain data using this type of calorimeter.

The experimental results, and related research, have also promoted application development.

In recent years, microchip calorimeters based on power-compensated dual sensors have attracted much attention in the field of microelectromechanical systems (MEMS) technology. Their wide range of applications...

This stems from three points. First, the scanning rate of traditional DSC cannot meet the research needs of rapid processes such as polymer phase transitions; second, FSC can characterize polymers...

The metastable microstructure of materials such as compounds; third, the widespread availability of commercial instruments with higher scanning rates and higher temperatures has further promoted the development of FSC.

The thermal history of the sample (especially the heating and cooling rates) and the processing technology can significantly alter the microstructure of the material, thus affecting its testing.

Performance deviates from its original state. The development of microelectromechanical system (MEMS) sensors has expanded the scan rate range and reduced the time constant, improving research...

Table 1 Typical test parameters for some chip calorimeters

FSC

Scan rate

Temperatures achievable at a constant rate purge gas Heating and cooling a Heating and cooling a Type mL/min Commercial Instruments 1 20000 5000 410 40 Nitrogen 20 20000 5000 410 140b Nitrogen 20 20000 5000.200 -25 Helium 20 Commercial Instruments 2 50000.20000 950 100 Nitrogen 20 50000.20000 950 250b Nitrogen 20 University self-assembled instruments 1000000 1000000 1000 30 Helium 0 (static atmosphere) 1000000 1000000 1000 -180 Helium 0 (static atmosphere) the cooling rate is determined by environmental conditions such as the temperature difference between the cooling device and the reference temperature, the heat flow rate, and the thermal conductivity of the purge gas.

b. Without cooling accessories.

Chip calorimetry

1 Scope

This document describes a method for thermal analysis using rapid differential scanning calorimetry (FSC) under non-adiabatic conditions, with the sample in an open state.

The placement method involves direct placement on the surface of the measurement area of a chip sensor based on microelectromechanical systems (MEMS) film technology, without crucible packaging. This document confirms...

The principle of rapid differential scanning calorimetry (FSC) for thermal analysis was established, and the conditioning and calibration of the testing instruments, samples, test environment and conditions were specified.

Requirements regarding accuracy, test procedures, characterization of physicochemical effects, heat capacity determination, of sample mass, precision and deviation, and test reports.

Due to the limitations of open sample placement methods, this document is only applicable to samples with a mass not exceeding 1 µg.

Note 1.Preparing samples with the smallest possible thickness helps to suppress the generation of high temperature gradients.

Note 2.Under heating and cooling modes, ultra-high-speed thermal scanning on the order of 10³ K/s and above can be achieved for tiny samples (mass <= 1 µg). This is achieved by reducing the sample size.

Quality and thickness can further improve scanning speed.

Note 3.Typically, the low scan rate of the FSC instrument overlaps with the high scan rate of the conventional differential scanning calorimetry (DSC) method in GB/T 19466.1, therefore it can be compared with the conventional method.

The results are correlated with the statistical DSC results.

This document applies to rapid kinetic effects of polymers, polymer blends, and composites (with or without fillers, fibers, or reinforcements).

Thermal analysis, including.

---Thermoplastics (polymers, molding blends, and other molding materials);

---Thermosetting plastics (uncured or cured materials);

---Elastomer.

This document describes qualitative and quantitative analysis methods for rapid physical and chemical processes in solid/liquid materials under varying heat flux rates, used for measurement...

Determining characteristic temperature and thermal effect, suitable for research.

---Metastable states and related processes (such as structural rearrangement, crystallization/recrystallization, annealing, aging, and amorphization);

---Chemical reactions (such as hydration, oxidation, polymerization, crosslinking, curing, and decomposition of elastomers and thermosetting plastics);

---Isothermal measurements of rapid crystallization systems or chemical reactions.

This document also applies to.

---Determination of heat capacity and study of changes in thermodynamic functions;

---Analysis of the thermal behavior of materials under rapidly changing temperature industrial process conditions;

---Separation of overlapping thermal effects from different kinetics (including interference-free analysis of melting and decomposition, glass transition and cold crystallization, and...) (Research on recombination of amorphous/semi-crystalline polymers via temperature-dependent rate changes).

2 Normative references

The contents of the following documents, through normative references within the text, constitute essential provisions of this document. Dated citations are not included.

For references to documents, only the version corresponding to that date applies to this document; for undated references, the latest version (including all amendments) applies.

This document.

GB/T 2035 Plastics Terminology GB/T 19466.1 Differential Scanning Calorimetry (DSC) for Plastics – Part 1: General Rules (GB/T 19466.1-2025) ISO 11357-1:2023, MOD)