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GB/T 40271-2021Test method for identification of textile fibers—Differential scanning calorimetry (DSC) (English PDF)

纺织纤维鉴别试验方法 差示扫描量热法(DSC)

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

May 21, 2021

Implementation date

December 1, 2021

Scope

GB/T 40271-2021 is the English-translated version of 纺织纤维鉴别试验方法 差示扫描量热法(DSC).

GB/T 40271-2021 describes how differential scanning calorimetry (DSC) is used to help identify textile fibres. It applies to fibres that show a clear melting peak below their decomposition temperature, and the method supports other identification tests rather than being used alone.

The DSC curve of the fibre is recorded and its melting peak temperature and enthalpy of fusion are read from it, since different synthetic fibres melt at different temperatures.

The standard covers equipment and materials, the sample, the heating programme - normally 10 °C/min from at least 50 °C below the melting peak - result expression and the test report, with annexes on temperature and heat calibration, standard samples and the melting data of synthetic fibres. It was issued on 21 May 2021 and has applied since 1 December 2021.

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Document preview — GB/T 40271-2021

National Standard of the People's Republic of China

ICS
59.080.01
Classification
W 04

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope4
  • 2 Normative References4
  • 3 Terms and Definitions4
  • 4 Test Principle5
  • 5 Equipment and Materials6
  • 6 Sample7
  • 7 Test Procedures7
  • 8 Result Expression8
  • 9 Test Report9
  • Appendix A (informative) Calibration Method10
  • Appendix B (informative) Standard Samples11
  • Appendix C (informative) Melting Peak Temperature and Enthalpy of Fusion of Synthetic Fibers12
  • Bibliography13

1 Scope

This Standard describes a test method for the identification of textile fibers through a differential scanning calorimeter.

This Standard is applicable to textile fibers with an obvious melting peak temperature, which is lower than decomposition temperature.

NOTE: the differential scanning calorimetry is generally not used alone, but by determining the melting peak temperature and enthalpy of fusion of fibers to assist in the identification of the fibers.

2 Normative References

The content of the following documents constitutes indispensable clauses of this document through normative references in the text. In terms of references with a specified date, only versions with a specified date are applicable to this document. In terms of references without a specified date, the latest version (including all the modifications) is applicable to this document.

FZ/T 01057.1 Test Method for Identification of Textile Fibers - Part 1: General

3 Terms and Definitions

The following terms and definitions are applicable to this document.

3.1 Melting

Melting refers to the transition from a solid state of a completely crystalline or partially crystalline substance to a liquid state with different viscosities. [source: GB/T 6425-2008, 3.5.5.1]

3.2 Enthalpy of Fusion

Enthalpy of fusion refers to the quantity of heat required for material melting under a constant pressure.

NOTE: it is expressed in kJ/kg or J/g. [source: GB/T 19466.3-2004, 3.3, modified]

3.3 Differential Scanning Calorimetry

Differential scanning calorimetry refers to a technique of determining the relationship between the heat flow rate or heating power (difference) delivered to the specimen and the reference substance, and temperature or time under program control temperature and certain atmosphere. [source: GB/T 6425-2008, 3.2.9]

3.4 Differential Scanning Calorimetry Curve (DSC curve)

Differential scanning calorimetry curve (DSC curve) refers to a graphical representation of the relationship curve between the heat flow rate or heating power (difference) delivered to the specimen and the reference substance measured by the differential scanning calorimeter, and temperature or time.

NOTE: the y-coordinate of the curve is heat flow rate, which is also known as heat flow and expressed in mW (mJ·s-1); the x-coordinate is temperature or time. [source: GB/T 6425-2008, 3.2.10, modified]

3.5 Calibration

Calibration refers to a set of operations of determining the relationship between the indicated value of the measuring instrument or measuring system and the already-known value corresponding to the measured value under specified conditions.

3.6 Instrument Baseline

Instrument baseline refers to a thermal analysis curve measured with empty sample cuvettes of the same mass and material, and without the use of specimen. [source: GB/T 6425-2008, 3.5.3.1 a), modified]

4 Test Principle

Under certain conditions, adopt the differential scanning calorimetry to determine and obtain the DSC curve of the fiber, as it is shown in Figure 1. In this Figure, Tpm is the melting peak temperature of the fiber; the connection points Tim and Tfm are used to draw a baseline; the area between it and the melting peak is the enthalpy of fusion of the fiber. Different types of synthetic fibers have different melting peak temperatures, based on which, the category of fibers can be identified.

7 Test Procedures

7.4 Take another sample cuvette (see 5.2); use the balance (see 5.4) to weigh its mass, accurate to 0.01 mg. Put the specimen into the sample cuvette; put on the cap and tightly seal it. Then, re-weigh the sample cuvette which holds the specimen, accurate to 0.01 mg.

7.5 Put the sample cuvette which holds the specimen into the sample holder at the designated position of the instrument; put the sealed empty sample cuvette into the other position as a reference.

7.6 Set the program of the instrument; deduct the instrument baseline. Under the condition of at least 50 °C lower than the melting peak temperature, at a rate of 10 °C/min, start to raise the temperature, until it is at least 30 °C higher than the extrapolated final temperature (Tefm), or 20 °C ~ 30 °C lower than the thermal decomposition temperature; record the DSC curve. For some new types of fibers and some fibers obtained through certain special processing, they may be heated up for the first time to eliminate the thermal history of the fiber processing process, then, heated up again for the observation of the DSC curve.

NOTE: other temperature-raising rates may also be adopted; the temperature-raising rate should not exceed 20 °C/min.

7.7 Cool down the instrument to room temperature; take out the sample cuvette; observe whether the sample cuvette is deformed, or whether the specimen overflows.

If it is found that the sample cuvette is deformed or the specimen overflows, then, the test shall be invalidated and re-conducted.

7.8 Repeat steps 7.4 ~ 7.7 to test the other two specimens.

8 Result Expression

8.1 Melting Peak Temperature

The test curve of the melting peak temperature is shown in Figure 1. From the Figure, respectively read the melting peak temperature (Tpm) of each specimen; the result shall be accurate to 0.1 °C. Take the average value of all specimens as the melting peak temperature of the sample; the result shall be rounded off to an integer. If the second temperature-raising is performed, take the value measured after the second temperature-raising as the test result. The melting peak temperature of synthetic fibers is shown in Appendix C.

8.2 Enthalpy of Fusion

The test curve of the enthalpy of fusion is shown in Figure 1. Take the area between […]

Appendix A (informative) Calibration Method

A.1 General Rules of Calibration

The differential scanning calorimeter is a sensitive thermal analysis instrument, which requires regular temperature and heat calibration. Under the circumstances of changing test temperature range, changing air source and flow rate, changing refrigeration system or being idle for a long time, before use, at least two standard samples shall be used for the calibration of temperature and heat. See Appendix B for commonly used standard samples.

NOTE: other calibration requirements of the instrument may comply with the recommendations by the manufacturer, or with the assistance of the manufacturer in the implementation.

A.2 Temperature Calibration

A.2.1 Select at least two standard samples with the same mass as the specimen to be tested and whose extrapolated initial temperature is at or close to the temperature range to be tested.

A.2.2 Under the same test conditions as the specimen to be tested, determine the extrapolated initial temperature of the standard samples and record it.

A.2.3 By comparing the standard value and the recorded value of the standard samples, determine the temperature correction coefficient for calibration. Alternatively, the computer system may automatically compare and calibrate in accordance with the standard value and the recorded value.

A.3 Heat Calibration

A.3.1 Select at least two standard samples with the same mass as the specimen to be tested and whose extrapolated initial temperature is at or close to the temperature range to be tested.

A.3.2 Under the same test conditions as the specimen to be tested, determine the enthalpy of fusion of the standard samples and record it.

A.3.3 By comparing the standard value and the recorded value of the standard samples, determine the heat correction coefficient for calibration. Alternatively, the computer system may automatically compare and calibrate in accordance with the standard value and the recorded value. […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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