E37.01 - Calorimetry and Mass Loss
Calorimetry and Mass Loss
General Information
SIGNIFICANCE AND USE
5.1 Vapor pressure is a fundamental thermodynamic property of a liquid. Vapor pressure and boiling temperature data are required for safety data sheets (SDS), the estimation of volatile organic compounds (VOC), and other needs related to product safety. Vapor pressures are important for prediction of the transport of a chemical in the environment; see Test Method E1194.
SCOPE
1.1 This test method describes procedures for determination of the vapor pressure of liquids by ebulliometry (boiling point measurements). It applies to pure liquids and azeotropes with an atmospheric boiling point between 285 K and 575 K, which can be condensed completely and returned to the ebulliometer boiler, that is, all materials must be condensable at total reflux. Liquid mixtures may be studied if they do not contain non-condensable components. Liquid mixtures that contain trace amounts of volatile but completely condensable components may also be studied, but they will produce vapor pressure data of greater uncertainty. Boiling point temperatures are measured at applied pressures of 1.0 kPa to 100 kPa (7.5 torr to 760 torr).
1.2 SI units are the standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method is useful in determining the extrapolated onset temperature, the peak heat flow temperature and the heat of reaction of a material. Any onset temperature determined by this test method is not valid for use as the sole information used for determination of storage or processing conditions.
5.2 This test method is useful in determining the fraction of a reaction that has been completed in a sample prior to testing. This fraction of reaction that has been completed can be a measure of the degree of cure of a thermally reactive polymer or can be a measure of decomposition of a thermally reactive material upon aging.
5.3 The heat of reaction values may be used in Practice E1231 to determine hazard potential figures-of-merit Explosion Potential and Shock Sensitivity.
5.4 This test method may be used in research, process control, quality assurance, and specification acceptance.
SCOPE
1.1 This test method determines the exothermic heat of reaction of thermally reactive chemicals or chemical mixtures, using milligram specimen sizes, by differential scanning calorimetry. Such reactive materials may include thermally unstable or thermoset materials.
1.2 This test method also determines the extrapolated onset temperature and peak heat flow temperature for the exothermic reaction.
1.3 This test method may be performed on solids, liquids or slurries.
1.4 The applicable temperature range of this test method is 25 °C to 600 °C.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard is related to Test Method E537, but provides additional information.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
6.1 These test methods are useful for research and development, quality assurance, regulatory compliance, and specification acceptance purposes.
6.2 The determination of the order of a chemical reaction or transformation at specific temperatures or time conditions is beyond the scope of these test methods.
6.3 The activation energy results obtained by these test methods may be compared with those obtained from Test Method E698 for nth order and accelerating reactions. Activation energy, pre-exponential factor, and reaction order results by these test methods may be compared to those for Test Method E2041 for nth order reactions.
SCOPE
1.1 Test Methods A, B, and C determine kinetic parameters for activation energy, pre-exponential factor and reaction order using differential scanning calorimetry (DSC) from a series of isothermal experiments over a small (≈10 K) temperature range. Test Method A is applicable to low nth order reactions. Test Methods B and C are applicable to accelerating reactions such as thermoset curing or pyrotechnic reactions and crystallization transformations in the temperature range from 300 K to 900 K (nominally 30 °C to 630 °C). These test methods are applicable only to these types of exothermic reactions when the thermal curves do not exhibit shoulders, double peaks, discontinuities or shifts in baseline.
1.2 Test Methods D and E also determines the activation energy of a set of time-to-event and isothermal temperature data generated by this or other procedures
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Differential scanning calorimetry provides a rapid test method for determining changes in specific heat capacity in a homogeneous material. The glass transition is manifested as a step change in specific heat capacity. For amorphous and semicrystalline materials the determination of the glass transition temperature may lead to important information about their thermal history, processing conditions, stability, progress of chemical reactions, and mechanical and electrical behavior.
5.2 This test method is useful for research, quality control, and specification acceptance.
SCOPE
1.1 This test method covers the assignment of the glass transition temperatures of materials using differential scanning calorimetry or differential thermal analysis.
1.2 This test method is applicable to amorphous materials or to partially crystalline materials containing amorphous regions, that are stable and do not undergo decomposition or sublimation in the glass transition region.
1.3 The normal operating temperature range is from −120 °C to 500 °C. The temperature range may be extended, depending upon the instrumentation used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 ISO standards 11357–2 is equivalent to this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.
5.2 This test method can be used for estimating lifetimes of materials, using Practice E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 K to 1300 K (nominally 100 °C to 1000 °C). The temperature range may be extended depending on the instrumentation used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The sulfated ash value indicates the level of known metal-containing additives or impurities in an organic material. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates. Tin and zinc are converted to their oxides.
5.2 This test method may be used for research and development, specification acceptance, and quality assurance purposes.
SCOPE
1.1 This test method describes the determination of sulfated ash content (sometimes called residue-on-ignition) of organic materials by thermogravimetry. This test method converts common metals found in organic materials (such as sodium, potassium, lithium, calcium, magnesium, zinc, and tin) into their sulfate salts permitting estimation of their total content as sulfates or oxides. The range of this test method is from 0.1 % to 100 % metal content.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The kinetic parameters combined with the general rate law and the reaction enthalpy can be used for the determination of thermal hazard using Practice E1231 (1).4
SCOPE
1.1 This test method covers the determination of the overall kinetic parameters for exothermic reactions using the Flynn/Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior can be described by the Arrhenius equation and the general rate law.
1.3 Limitations—There are cases where this technique is not applicable. Limitations may be indicated by curves departing from a straight line (see 11.2) or the isothermal aging test not closely agreeing with the results predicted by the calculated kinetic values. In particular, this test method is not applicable to reactions that are partially inhibited. The technique may not work with reactions that include simultaneous or consecutive reaction steps. This test method may not apply to materials that undergo phase transitions if the reaction rate is significant at the transition temperature.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
6.1 This test method is useful in research and development.
6.2 The determination of the appropriate model for a chemical reaction or transformation and the values associated with its kinetic parameters may be used in the estimation of reaction performance at temperatures or time conditions not easily tested. This use, however, is not described in this test method.
SCOPE
1.1 This test method describes the determination of the kinetic parameters of activation energy, Arrhenius pre-exponential factor, and reaction order using the Borchardt and Daniels2 treatment of data obtained by differential scanning calorimetry. This test method is applicable to the temperature range from 170 K to 870 K (−100 °C to 600°C).
1.2 This treatment is applicable only to smooth exothermic reactions with no shoulders, discontinuous changes, or shifts in baseline. It is applicable only to reactions with reaction order n ≤ 2. It is not applicable to acceleratory reactions and, therefore, is not applicable to the determination of kinetic parameters for most thermoset curing reactions or to crystallization reactions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Oxidative induction time is a relative measure of the degree of oxidative stability of the material evaluated at the isothermal temperature of the test. The presence, quantity or effectiveness of antioxidants may be determined by this method. The OIT values thus obtained may be compared from one hydrocarbon to another or to a reference material to obtain relative oxidative stability information.
5.2 Typical uses include the oxidative stability of edible oils and fats (oxidative rancidity), lubricants, greases, and polyolefins.
SCOPE
1.1 These test methods describe the determination of the oxidative properties of hydrocarbons by differential scanning calorimetry or pressure differential scanning calorimetry and is applicable to hydrocarbons that oxidize exothermically in their analyzed form.
1.2 Test Method A—A differential scanning calorimeter (DSC) is used at ambient pressure, for example, about 100 kPa of oxygen.
1.3 Test Method B—A pressure DSC (PDSC) is used at high pressure, for example, 3.5 MPa (500 psig) oxygen.
1.4 Units—The values stated in SI units are to be regarded as standard. Imperial units are provided for user convenience and are not the standard.
1.5 These test methods are related to ISO 11357–6 but is different in technical content. These test methods are related to CEC L-85–T but includes additional experimental conditions.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in 7.4 and 12.10.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Modulated temperature differential scanning calorimetric measurements provide a rapid, simple method for determining specific heat capacities of materials, even under quasi-isothermal conditions.
5.2 Specific heat capacities are important for design purposes, quality control, and research and development.
5.3 The use of a stepped quasi-isothermal program may be used to follow structure changes in materials.
SCOPE
1.1 This test method describes the determination of specific heat capacity by modulated temperature differential scanning calorimetry. For the determination of specific heat capacity by a step-isothermal or multiple step-isothermal temperature program, the reader is referred to Test Method E1269.
1.2 This test method is generally applicable to thermally stable solids and liquids.
1.3 The normal operating range of the test is from (–100 to 600) °C. The temperature range may be extended depending upon the instrumentation and specimen holders used.
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Oxidation onset temperature is a relative measure of the degree of oxidative stability of the material evaluated at a given heating rate and oxidative environment (e.g., oxygen); the higher the OOT value the more stable the material. The OOT is described in Fig. 1. The OOT values can be used for comparative purposes and are not an absolute measurement, like the oxidation induction time (OIT) at a constant temperature (see Test Method E1858). The presence or effectiveness of antioxidants may be determined by these test methods.
FIG. 1 DSC Oxidation (Extrapolated) Onset Temperature (OOT)
5.2 Typical uses of these test methods include the oxidative stability of edible oils and fats (oxidative rancidity), lubricants, greases, and polyolefins.
SCOPE
1.1 These test methods describe the determination of the oxidative properties of hydrocarbons by differential scanning calorimetry or pressure differential scanning calorimetry under linear heating rate conditions and are applicable to hydrocarbons, which oxidize exothermically in their analyzed form.
1.2 Test Method A—A differential scanning calorimeter (DSC) is used at ambient pressure of one atmosphere of oxygen.
1.3 Test Method B—A pressure DSC (PDSC) is used at high pressure (e.g., 3.5 MPa (500 psig) of oxygen).
1.4 Test Method C—A differential scanning calorimeter (DSC) is used at ambient pressure of one atmosphere of air.
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Vapor pressure is a fundamental thermophysical property of a liquid. Vapor pressure data are useful in process design and control, in establishing environmental regulations for safe handling and transport, for estimation of volatile organic content (VOC), and in deriving hazard assessments. Vapor pressure and boiling temperature data are required for Safety Data Sheets (SDS). The enthalpy of vaporization may also be estimated from the slope of the vapor pressure curve (see Practice E2071).
SCOPE
1.1 This test method describes a procedure for the determination of the vapor pressure of pure liquids or melts from boiling point measurements made using differential thermal analysis (DTA) or differential scanning calorimetry (DSC) instrumentation operated at different applied pressures.
1.2 This test method can be used for the temperature range 273 K to 773 K (0 °C to 500 °C) and for pressures between 0.2 kPa to 2 MPa. These ranges may differ depending upon the instrumentation used and the thermal stability of materials tested. Because a range of applied pressures is required by this test method, the analyst is best served by use of instrumentation referred to as high pressure differential thermal instrumentation (HPDSC or HPDTA).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. (See also IEEE/ASTM SI 10.)
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.
5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.
SCOPE
1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1 mg to 3 mg specimen sizes over the temperature range from ambient to 600 °C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the glass transition.
5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity.
5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events making it possible to determine the glass transition in the presence of interfering kinetic event.
5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance.
5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356), thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640).
SCOPE
1.1 These test methods describe the assignment of the glass transition temperature of materials using modulated temperature differential scanning calorimetry (MTDSC) over the temperature range from –120 °C to +600 °C. The temperature range may be extended depending upon the instrumentation used.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
6.1 This test method is useful for research and development, quality assurance, regulatory compliance and specification-based acceptance.
6.2 The kinetic parameters determined by this method may be used to calculate thermal hazard figures-of-merit according to Practice E1231.
SCOPE
1.1 This test method describes the determination of the kinetic parameters of Arrhenius activation energy and pre-exponential factor using the Kissinger variable heating rate iso-conversion method (1, 2)2 and activation energy and reaction order by the Farjas method (3) for thermally unstable materials. The test method is applicable to the temperature range from 300 K to 900 K (27 °C to 627 °C).
1.2 Both nth order and accelerating reactions are addressed by this method over the range of 0.5 n p n is the nth order reaction order and p is the Avrami reaction order (4). Reaction orders n and p are determined by the Farjas method (3).
1.3 This test method uses the same experimental conditions as Test Method E698. The Flynn/Wall/Ozawa data treatment of Test Method E698 may be simultaneously applied to these experimental results.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the thermal decomposition and reaction mass change of a material.
5.2 This test method is useful in detecting potentially hazardous reactions and in estimating the temperatures at which these reactions occur. This test method is recommended as a screening test for detecting the thermal hazards of an uncharacterized material or mixture (see Section 8).
5.3 Energetic materials, pharmaceuticals and polymers are examples of materials for which this test might be useful. This test is especially useful for materials having melting points that overlap with the onset of reaction or decomposition.
Note 1: In differential scanning calorimetry (DSC), the melting endotherm may interfere with the determination of the onset temperature for reaction or decomposition.
5.4 This test is not suitable for materials that sublime or vaporize in the temperature range of interest. A sample with volatile impurities needs to be purified prior to testing by thermogravimetric analysis. Alternatively, the sample can be tested as is, however, special caution is required during the data analysis. The mass loss due to the loss of impurity should not interfere with the determination of reaction or decomposition temperature.
5.5 The four significant criteria of this test method are: the detection of a sample mass change; the extent of the mass change; the approximate temperature at which the event occurs; the observance of effects due to the atmosphere.
SCOPE
1.1 This test method describes the assessment of material thermal stability through the determination of the temperature at which the materials start to decompose or react and the extent of the mass change using thermogravimetry. The test method uses minimum quantities of material and is applicable over the temperature range from ambient to 800 °C.
1.2 The absence of reaction or decomposition is used as an indication of thermal stability in this test method under the experimental conditions used.
1.3 This test method may be performed on solids or liquids, which do not sublime or vaporize in the temperature range of interest.
1.4 This test method shall not be used by itself to establish a safe operating or storage temperature. It may be used in conjunction with other test methods (for example, Test Methods E487 and E537, and Guide E1981) as part of a hazard analysis of a material.
1.5 This test method is normally applicable to reaction or decomposition occurring in the range from room temperature to 800 °C. The temperature range may be extended depending on the instrumentation used.
1.6 This test method may be performed in an inert, a reactive or self-generated atmosphere.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The activation energy may be used to calculate thermal endurance and an estimate of the lifetime of the material at specified temperatures using Test Method E1877.
5.2 The kinetic parameters determined by these test methods may be used in quality assurance, specification acceptance, research, and development.
5.3 The kinetic parameters of activation energy and logarithm of the pre-exponential factor determined by these test methods have little intrinsic value in themselves. Most practical applications of this information, such as lifetime estimation (see Test Method E1877), also require an estimation of the precision of the respective values. Determination of that precision by replicated determination is a non-manditory part of these test methods.
SCOPE
1.1 These test methods describe the model-free determination of Arrhenius activation energy by thermogravimetry using the factor jump (1)2 (Test Method A) or modulated thermogravimetry (2) (Test Methods B and C) techniques. With the assumption of a first-order kinetic model, the pre-exponential factor is additionally determined.
1.2 These test methods are applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change.
1.3 These test methods are applicable to decomposition occurring in the range from 400 K to 1200 K (nominally 100 °C to 900 °C). The temperature range may be extended depending on the instrumentation and material used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetric analyzers are used to characterize a broad range of materials. In most cases, one of the desired values to be assigned in thermogravimetric measurements is the temperature at which significant changes in specimen mass occur. Therefore, the temperature axis (abscissa) of all apparent-mass-change curves must be calibrated accurately, either by direct reading of a temperature sensor, or by adjusting the programmer temperature to match the actual temperature over the temperature range of interest. In the latter case, this is accomplished by the use of either melting point or magnetic transition standards.
5.2 This test method permits interlaboratory comparison and intralaboratory correlation of instrumental temperature scale data.
SCOPE
1.1 This test method describe the temperature calibration of thermogravimetric analyzers over the temperature range from 25 °C to 1500 °C and is applicable to commercial and custom-built apparatus. This calibration may be accomplished by the use of either melting point standards or magnetic transition standards.
1.2 The weight change curve in thermogravimetry results from a number of influences, some of which are characteristic of the specimen holder assembly and atmosphere rather than the specimen. The variations from instrument to instrument occur in the point of measurement of the temperature, the nature of the material, its size and packing, the geometry and composition of the specimen container, the geometry and design of the furnace, and the accuracy and sensitivity of the temperature sensor and displaying scales. These all contribute to differences in measured temperatures, which may exceed 20 °C. In addition, some sample holder assemblies will show variations of measured temperature with sample size or heating/cooling rate, or both. Since it is neither practical nor advisable to standardize sample holders or thermobalance geometries, instruments may be calibrated by measurement of the deviation of a melting or magnetic (Curie point) transition temperature from the standard reference temperature. This deviation can be applied as a correction term to subsequent measurements.
1.3 This test method assumes that the indicated temperature of the instrument is linear over the range defined by a two-point calibration and that this linearity has been verified. These two calibration temperatures should be as close to the experimental measurements to be made as possible.
1.4 This test method describes two procedures for temperature calibration of thermogravimetric analyzers using any type balance. Procedure A uses melting point standards for calibration. Procedure B uses magnetic transition standards for calibration.
1.5 The data generated by these procedures can be used to correct the temperature scale of the instrument by either a positive or negative amount using either a one- or two-point temperature calibration procedure.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Volatility of a material is not an equilibrium thermodynamic property but is a characteristic of a material related to a thermodynamic property that is vapor pressure. It is influenced by such factors as surface area, temperature, particle size, and purge gas flow rate; that is, it is diffusion controlled.
5.2 The extent of containment achieved for specimens in these test methods by means of a pinhole opening between 0.33 mm to 0.38 mm allows for measurement circumstances that are relatively insensitive to experimental variables other than temperature. Decreasing the extent of containment by use of pinholes larger than 0.38 mm will increase the magnitude of the observed rate of mass loss but will also reduce the measurement precision by increasing the sensitivity to variations in other experimental variables.
5.3 Results obtained by these test methods are not strictly equivalent to those experienced in processing or handling conditions but may be used to rank materials for their volatility in such circumstances. Therefore, the volatility rates determined by these test methods should be considered as index values only.
5.4 The volatility rate may be used to estimate such quantifiable values as drying interval or the extent of volatile release from a process.
SCOPE
1.1 These test methods cover procedures for assessing the volatility of solids and liquids at given temperatures using thermogravimetry under prescribed experimental conditions. Results of these test methods are obtained as volatility rates expressed as mass per unit time. Rates ≥5 μg/min are achievable with these test methods.
1.2 Temperatures typical for these test methods are within the range from 25 °C to 500 °C. This temperature range may differ depending upon the instrumentation used.
1.3 These test methods are intended to provide a value for the volatility rate of a sample using a thermogravimetric analysis measurement on a single representative specimen. It is the responsibility of the user of these test methods to determine the need for and the number of repetitive measurements on fresh specimens necessary to satisfy end use requirements.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 These test methods are used to estimate the amount of volatile materials present in a material.
5.2 These test methods are useful for design purposes, service evaluation, regulatory statutes, manufacturing control, quality control, specification acceptance, development, and research.
5.3 The results obtained by these test methods may be equivalent to those obtained by other test methods and may be known by other terms in their respective fields. Other tests and terms encountered include loss-on-heating (see Footnote 5 and Test Methods D6, D2288, and E359); heating loss (see Test Methods D1509); evaporative loss (see Test Method D2595); volatile organic carbon, moisture, or water (see Test Methods D2216 and D3175); volatility (see Test Method D4893); highly volatile matter (see Test Method E897); and volatile content (see Guide D2832).
SCOPE
1.1 These test methods describe a procedure for determining the amount of volatile matter of any kind that is driven off from a test specimen under a specific set of temperature and time conditions. These test methods determine only the mass of material lost, not its identity.
1.2 These test methods are applicable to a wide variety of solid or liquid materials, mixtures, or blends where the major component is stable at the test temperature.
Note 1: These test methods can be applied to the analysis of volatile organic compounds (VOC) content in metalworking fluids and direct contact lubricants subject to South Coast Air Quality Management District (SCAQMD) Rule 1144.
1.3 The applicable temperature range for these test methods are generally between ambient temperature and 1000°C.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 There is no ISO method equivalent to this test standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method is intended for use in quality control, material screening, and related problem solving where a compositional analysis is desired or a comparison can be made with a known material of the same type.
5.2 The parameters described should be considered as guidelines. They may be altered to suit a particular analysis, provided the changes are noted in the report.
5.3 The proportion of the determined components in a given mixture or blend may indicate specific quality or end use performance characteristics. Particular examples include the following:
5.3.1 Increasing soot (carbon) content of used diesel lubricating oils indicates decreasing effectiveness.
5.3.2 Specific carbon-to-polymer ratio ranges are required in some elastomeric and plastic parts in order to achieve desired mechanical strength and stability.
5.3.3 Some filled elastomeric and plastic products require specific inert content (for example, ash, filler, reinforcing agent, etc.) to meet performance specifications.
5.3.4 The volatile matter, fixed carbon, and ash content of coal and coke are important parameters. The “ranking” of coal increases with increasing carbon content and decreasing volatile and hydrocarbon, (medium volatility) content.
SCOPE
1.1 This test method provides a general technique incorporating thermogravimetry to determine the amount of highly volatile matter, medium volatile matter, combustible material, and ash content of compounds. This test method will be useful in performing a compositional analysis in cases where agreed upon by interested parties.
1.2 This test method is applicable to solids and liquids.
1.3 The temperature range of test is typically room temperature to 1000 °C. Composition between 1 weight % and 100 weight % of individual components may be determined.
1.4 This test method utilizes an inert and reactive gas environment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method calibrates or demonstrates conformity of thermogravimetric apparatus at ambient conditions. Most thermogravimetry analysis experiments are carried out under temperature ramp conditions or at isothermal temperatures distant from ambient conditions. This test method does not address the temperature effects on mass calibration.
5.2 In most thermogravimetry experiments, the mass change is reported as weight percent in which the observed mass at any time during the course of the experiment is divided by the original mass of the test specimen. This method of reporting results assumes that the mass scale of the apparatus is linear with increasing mass. In such cases, it may be necessary only to confirm the performance of the instrument by comparison to a suitable reference.
5.3 When the actual mass of the test specimen is recorded, the use of a calibration factor to correct the calibration of the apparatus may be required, on rare occasions.
SCOPE
1.1 This test method describes the calibration or performance confirmation of the mass (or weight) scale of thermogravimetric analyzers and is applicable to commercial and custom-built apparatus.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard3 pagesEnglish language
- Standard3 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method is useful in calibrating the temperature signal of a DSC for cooling experiments such as the determination of crystallization temperatures in Test Method D3418 and Test Method E794.
5.2 This test method may be used for research, development, analytical, specification acceptance, quality assurance, and control purposes.
SCOPE
1.1 This test method describes the temperature calibration of differential scanning calorimeters (DSCs) on cooling using the difference between transition temperatures upon heating and cooling in the temperature range of 65 °C to 420 °C. An offset in the indicated temperature between heating and cooling experiments, within this temperature range, may be used to provide temperature calibration on cooling at other temperature ranges.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Test Method E3142 is an alternative to this test method.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The melting temperature range of a compound broadens as the impurity level rises. This phenomenon is described approximately by the van’t Hoff equation for melting point depressions. Measuring and recording the instantaneous heat flow into the specimen as a function of temperature during such a melting process is a practical way for the generation of data suitable for analysis by the van’t Hoff equation.
5.2 The results obtained include: sample purity (expressed as mole percent); enthalpy of fusion (expressed as J/mol); and the melting temperature (expressed in Kelvin) of the pure form of the major component.
5.3 Generally, the repeatability of this test method decreases as the purity level decreases. This test method is ordinarily considered unreliable when the purity level of the major component of the mixture is less than 98.5 mol % or when the incremental enthalpy correction (c) exceeds 20 % of the original detected enthalpy of fusion.
5.4 This test method is used for quality control, specification acceptance, and research.
SCOPE
1.1 This test method describes the determination of purity of materials greater than 98.5 mole percent purity using differential scanning calorimetry and the van’t Hoff equation.
1.2 This test method is applicable to thermally stable compounds with well-defined melting temperatures.
1.3 Determination of purity by this test method is only applicable when the impurity dissolves in the melt and is insoluble in the crystal.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Differential scanning calorimetry provides a rapid method for the determination of enthalpic changes accompanying first-order transitions of materials.
5.2 This test method is useful for quality control, specification acceptance, and research.
SCOPE
1.1 This test method describes the determination of the enthalpy (heat) of fusion (melting) and crystallization by differential scanning calorimetry (DSC).
1.2 This test method is applicable to solid samples in granular form or in any fabricated shape from which an appropriate specimen can be cut, or to liquid samples that crystallize within the range of the instrument. Note, however, that the results may be affected by the form and mass of the specimen, as well as by other experimental conditions.
1.3 The normal operating temperature range is from −120 to 600°C. The temperature range can be extended depending upon the instrumentation used.
1.4 This test method is generally applicable to thermally stable materials with well defined endothermic or exothermic behavior.
1.5 Computer or electronic based instruments, techniques, or data treatment equivalent to those in this test method may also be used.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 The enthalpy of melting and crystallization portion of ISO 11357-3 is equivalent to this standard.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Differential scanning calorimetric measurements provide a rapid, simple method for determining specific heat capacities of materials.
5.2 Specific heat capacities are important for reactor and cooling system design purposes, quality control, and research and development.
SCOPE
1.1 This test method covers the determination of specific heat capacity by differential scanning calorimetry.
1.2 This test method is generally applicable to thermally stable solids and liquids.
1.3 The normal operating range of the test is from − 100 to 600°C. The temperature range can be extended, depending upon the instrumentation and specimen holders used.
1.4 Computer or electronic-based instrumentation, techniques, or data treatment equivalent to this test method may be used.
Note 1: Users of this test method are expressly advised that all such instruments or techniques may not be equivalent. It is the responsibility of the user of this test method to determine equivalency prior to use.
1.5 This test method is similar to ISO 11357–4, but contains additional methodology not found in that method. Additionally, ISO 11357–4 contains practices not found in this standard. This test method is similar to Japanese Industrial Standard K 7123, but contains additional methodology not found in that method.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Differential scanning calorimetry and differential thermal analysis provide a rapid method for determining the fusion and crystallization temperatures of crystalline materials.
5.2 This test is useful for quality control, specification acceptance, and research.
SCOPE
1.1 This test method describes the determination of melting (and crystallization) temperatures of pure materials by differential scanning calorimetry (DSC) and differential thermal analysis (DTA).
1.2 This test method is generally applicable to thermally stable materials with well-defined melting temperatures.
1.3 The normal operating range is from −120 to 600°C for DSC and 25 to 1500°C for DTA. The temperature range can be extended depending upon the instrumentation used.
1.4 Computer or electronic based instruments, techniques, or data treatment equivalent to those in this test method may be used.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Differential scanning calorimeters and differential thermal analyzers are used to determine the transition temperatures of materials. For this information to be meaningful in an absolute sense, temperature calibration of the apparatus and comparison of the resulting data to that of known standard materials is required.
5.2 This test method is useful in calibrating the temperature axis of differential scanning calorimeters and differential thermal analyzers.
SCOPE
1.1 This test method describes the temperature calibration of differential thermal analyzers and differential scanning calorimeters over the temperature range from −40°C to +2000°C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This test method is similar to ISO standard 11357–1.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Vapor pressure is a fundamental thermodynamic property of a liquid. Vapor pressure and boiling temperature data are required for material safety data sheets (MSDS), the estimation of volatile organic compounds (VOC), and other needs related to product safety. Vapor pressures are important for prediction of the transport of a chemical in the environment; see Test Method E1194.
SCOPE
1.1 This test method describes procedures for determination of the vapor pressure of liquids by ebulliometry (boiling point measurements). It is applicable to pure liquids and azeotropes that have an atmospheric boiling point between 285 and 575 K and that can be condensed completely and returned to the ebulliometer boiler, that is, all materials must be condensable at total reflux. Liquid mixtures may be studied if they do not contain non-condensable components. Liquid mixtures that contain trace amounts of volatile but completely condensable components may also be studied, but they will produce vapor pressure data of greater uncertainty. Boiling point temperatures are measured at applied pressures of 1.0 to 100 kPa (7.5 to 760 torr).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There is no ISO equivalent to this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.
5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.
SCOPE
1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1 mg to 3 mg specimen sizes over the temperature range from ambient to 600 °C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.
5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.
SCOPE
1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1–3 mg specimen sizes over the temperature range from ambient to 600 °C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The activation energy may be used to calculate thermal endurance and an estimate of the lifetime of the material at specified temperatures using Test Method E1877.
5.2 The kinetic parameters determine by these test methods may be used in quality assurance, specification acceptance, research, and development.
5.3 The kinetic parameters of activation energy and logarithm of the pre-exponential factor determined by these test methods have little intrinsic value in themselves. Most practical applications of this information, such as lifetime estimation (see Test Method E1877), also require an estimation of the precision of the respective values. Determination of that precision by replicated determination is a non-manditory part of these test methods.
SCOPE
1.1 These test methods describe the model-free determination of Arrhenius activation energy by thermogravimetry using the factor jump (1)2 (Test Method A) or modulated thermogravimetry (2) (Test Methods B and C) techniques. With the assumption of a first-order kinetic model, the pre-exponential factor is additionally determined.
1.2 These test methods are applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change.
1.3 These test methods are applicable to decomposition occurring in the range from 400 K to 1200 K (nominally 100 °C to 900 °C). The temperature range may be extended depending on the instrumentation and material used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.
5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.
SCOPE
1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1–3 mg specimen sizes over the temperature range from ambient to 600 °C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.
5.2 This test method can be used for estimating lifetimes of materials, using Practice E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 K to 1300 K (nominally 100°C to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The kinetic parameters combined with the general rate law and the reaction enthalpy can be used for the determination of thermal hazard using Practice E1231 (1).3
SCOPE
1.1 This test method covers the determination of the overall kinetic parameters for exothermic reactions using the Flynn/Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior can be described by the Arrhenius equation and the general rate law.
1.3 Limitations—There are cases where this technique is not applicable. Limitations may be indicated by curves departing from a straight line (see 11.2) or the isothermal aging test not closely agreeing with the results predicted by the calculated kinetic values. In particular, this test method is not applicable to reactions that are partially inhibited. The technique may not work with reactions that include simultaneous or consecutive reaction steps. This test method may not apply to materials that undergo phase transitions if the reaction rate is significant at the transition temperature.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
6.1 These test methods are useful for research and development, quality assurance, regulatory compliance, and specification acceptance purposes.
6.2 The determination of the order of a chemical reaction or transformation at specific temperatures or time conditions is beyond the scope of these test methods.
6.3 The activation energy results obtained by these test methods may be compared with those obtained from Test Method E698 for nth order and accelerating reactions. Activation energy, pre-exponential factor, and reaction order results by these test methods may be compared to those for Test Method E2041 for nth order reactions.
SCOPE
1.1 Test Methods A, B, and C determine kinetic parameters for activation energy, pre-exponential factor and reaction order using differential scanning calorimetry from a series of isothermal experiments over a small ( ≈10 K) temperature range. Test Method A is applicable to low nth order reactions. Test Methods B and C are applicable to accelerating reactions such as thermoset curing or pyrotechnic reactions and crystallization transformations in the temperature range from 300 to 900 K (nominally 30 to 630°C). These test methods are applicable only to these types of exothermic reactions when the thermal curves do not exhibit shoulders, double peaks, discontinuities or shifts in baseline.
1.2 Test Methods D and E also determines the activation energy of a set of time-to-event and isothermal temperature data generated by this or other procedures
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 These test methods are similar but not equivalent to ISO DIS 11357, Part 5, and provides more information than the ISO standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
SIGNIFICANCE AND USE
6.1 This test method is useful for research and development, quality assurance, regulatory compliance and specification-based acceptance.
6.2 The kinetic parameters determined by this method may be used to calculate thermal hazard figures-of-merit according to Practice E1231.
SCOPE
1.1 This test method describes the determination of the kinetic parameters of Arrhenius activation energy and pre-exponential factor using the Kissinger variable heating rate iso-conversion method (1, 2)2 and activation energy and reaction order by the Farjas method (3) for thermally unstable materials. The test method is applicable to the temperature range from 300 to 900 K (27 to 627°C).
1.2 Both nth order and accelerating reactions are addressed by this method over the range of 0.5 n p n is the nth order reaction order and p is the Avrami reaction order (4). Reaction orders n and p are determined by the Farjas method (3).
1.3 This test method uses the same experimental conditions as Test Method E698. The Flynn/Wall/Ozawa data treatment of Test Method E698 may be simultaneously applied to these experimental results.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 There is no ISO equivalent to this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard11 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method is useful in determining the extrapolated onset temperature, the peak heat flow temperature and the heat of reaction of a material. Any onset temperature determined by this test method is not valid for use as the sole information used for determination of storage or processing conditions.
5.2 This test method is useful in determining the fraction of a reaction that has been completed in a sample prior to testing. This fraction of reaction that has been completed can be a measure of the degree of cure of a thermally reactive polymer or can be a measure of decomposition of a thermally reactive material upon aging.
5.3 The heat of reaction values may be used in Practice E1231 to determine hazard potential figures-of-merit Explosion Potential and Shock Sensitivity.
5.4 This test method may be used in research, process control, quality assurance, and specification acceptance.
SCOPE
1.1 This test method determines the exothermic heat of reaction of thermally reactive chemicals or chemical mixtures, using milligram specimen sizes, by differential scanning calorimetry. Such reactive materials may include thermally unstable or thermoset materials.
1.2 This test method also determines the extrapolated onset temperature and peak heat flow temperature for the exothermic reaction.
1.3 This test method may be performed on solids, liquids or slurries.
1.4 The applicable temperature range of this test method is 25 to 600°C.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 There is no ISO method equivalent to this standard.
1.7 This standard is related to Test Method E537 and to NAS 1613, but provides additional information.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
6.1 This test method is useful in research and development.
6.2 The determination of the appropriate model for a chemical reaction or transformation and the values associated with its kinetic parameters may be used in the estimation of reaction performance at temperatures or time conditions not easily tested. This use, however, is not described in this test method.
SCOPE
1.1 This test method describes the determination of the kinetic parameters of activation energy, Arrhenius pre-exponential factor, and reaction order using the Borchardt and Daniels2 treatment of data obtained by differential scanning calorimetry. This test method is applicable to the temperature range from 170 to 870 K (−100 to 600°C).
1.2 This treatment is applicable only to smooth exothermic reactions with no shoulders, discontinuous changes, or shifts in baseline. It is applicable only to reactions with reaction order n ≤ 2. It is not applicable to acceleratory reactions and, therefore, is not applicable to the determination of kinetic parameters for most thermoset curing reactions or to crystallization reactions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This test method is similar, but not equivalent to, ISO 11357, Part 5, that contains provisions for additional information not supplied by this test method.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The sulfated ash may be used to indicate the level of known metal-containing additives or impurities in an organic material. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates. Tin and zinc are converted to their oxides.
5.2 This test method may be used for research and development, specification acceptance, and quality assurance purposes.
SCOPE
1.1 This test method describes the determination of sulfated ash content (sometimes called residue-on-ignition) of organic materials by thermogravimetry. This test method converts common metals found in organic materials (such as sodium, potassium, lithium, calcium, magnesium, zinc, and tin) into their sulfate salts permitting estimation of their total content as sulfates or oxides. The range of this test method is from 0.1 to 100 % metal content.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard3 pagesEnglish language
- Standard3 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This test method is useful in calibrating the temperature signal of a differential scanning calorimeter for cooling experiments such as the determination of crystallization temperatures in Test Method D3418 and Test Method E794.
5.2 This test method may be used for research, development, analytical, specification acceptance, quality assurance, and control purposes.
SCOPE
1.1 This test method covers the temperature calibration of differential scanning calorimeters on cooling using the difference between transition temperatures upon heating and cooling in the temperature range of 50 to 185°C. An offset in the indicated temperature between heating and cooling experiments, within this temperature range, may be used to provide temperature calibration on cooling at other temperature ranges.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetric analyzers are used to characterize a broad range of materials. In most cases, one of the desired values to be assigned in thermogravimetric measurements is the temperature at which significant changes in specimen mass occur. Therefore, the temperature axis (abscissa) of all apparent-mass-change curves must be calibrated accurately, either by direct reading of a temperature sensor, or by adjusting the programmer temperature to match the actual temperature over the temperature range of interest. In the latter case, this is accomplished by the use of either melting point or magnetic transition standards.
5.2 This test method permits interlaboratory comparison and intralaboratory correlation of instrumental temperature scale data.
SCOPE
1.1 This test method describe the temperature calibration of thermogravimetric analyzers over the temperature range from 25 to 1500 °C and is applicable to commercial and custom-built apparatus. This calibration may be accomplished by the use of either melting point standards or magnetic transition standards.
1.2 The weight change curve in thermogravimetry results from a number of influences, some of which are characteristic of the specimen holder assembly and atmosphere rather than the specimen. The variations from instrument to instrument occur in the point of measurement of the temperature, the nature of the material, its size and packing, the geometry and composition of the specimen container, the geometry and design of the furnace, and the accuracy and sensitivity of the temperature sensor and displaying scales. These all contribute to differences in measured temperatures, which may exceed 20 °C. In addition, some sample holder assemblies will show variations of measured temperature with sample size or heating/cooling rate, or both. Since it is neither practical nor advisable to standardize sample holders or thermobalance geometries, instruments may be calibrated by measurement of the deviation of a melting or magnetic (Curie Point) transition temperature from the standard reference temperature. This deviation can be applied as a correction term to subsequent measurements.
1.3 This test method assumes that the indicated temperature of the instrument is linear over the range defined by a two-point calibration and that this linearity has been verified. These two calibration temperatures should be as close to the experimental measurements to be made as possible.
1.4 This test method describes two procedures for temperature calibration of thermogravimetric analyzers using any type balance. Procedure A uses melting point standards for calibration. Procedure B uses magnetic transition standards for calibration.
1.5 The data generated by these procedures can be used to correct the temperature scale of the instrument by either a positive or negative amount using either a one- or two-point temperature calibration procedure.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the thermal decomposition and reaction mass change of a material.
5.2 This test method is useful in detecting potentially hazardous reactions and in estimating the temperatures at which these reactions occur. This test method is recommended as a screening test for detecting the thermal hazards of an uncharacterized material or mixture (see Section 8).
5.3 Energetic materials, pharmaceuticals and polymers are examples of materials for which this test might be useful. This test is especially useful for materials having melting points that overlap with the onset of reaction or decomposition.
Note 1: In Differential Scanning Calorimetry (DSC), the melting endotherm may interfere with the determination of the onset temperature for reaction or decomposition.
5.4 This test is not suitable for materials that sublime or vaporize in the temperature range of interest. A sample with volatile impurities needs to be purified prior to testing by thermogravimetric analysis. Alternatively, the sample can be tested as is, however, special caution is required during the data analysis. The mass loss due to the loss of impurity should not interfere with the determination of reaction or decomposition temperature.
5.5 The four significant criteria of this test method are: the detection of a sample mass change; the extent of the mass change; the approximate temperature at which the event occurs; the observance of effects due to the atmosphere.
SCOPE
1.1 This test method describes the assessment of material thermal stability through the determination of the temperature at which the materials start to decompose or react and the extent of the mass change using thermogravimetry. The test method uses minimum quantities of material and is applicable over the temperature range from ambient to 800°C.
1.2 The absence of reaction or decomposition is used as an indication of thermal stability in this test method under the experimental conditions used.
1.3 This test method may be performed on solids or liquids, which do not sublime or vaporize in the temperature range of interest.
1.4 This test method shall not be used by itself to establish a safe operating or storage temperature. It may be used in conjunction with other test methods (for example, Test Methods E487 and E537, and Guide E1981) as part of a hazard analysis of a material.
1.5 This test method is normally applicable to reaction or decomposition occurring in the range from room temperature to 800°C. The temperature range may be extended depending on the instrumentation used.
1.6 This test method may be performed in an inert, a reactive or self-generated atmosphere.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health and environmental practices and determine the applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Volatility of a material is not an equilibrium thermodynamic property but is a characteristic of a material related to a thermodynamic property that is vapor pressure. It is influenced by such factors as surface area, temperature, particle size, and purge gas flow rate; that is, it is diffusion controlled.
5.2 The extent of containment achieved for specimens in these test methods by means of a pinhole opening between 0.33 mm to 0.38 mm allows for measurement circumstances that are relatively insensitive to experimental variables other than temperature. Decreasing the extent of containment by use of pinholes larger than 0.38 mm will increase the magnitude of the observed rate of mass loss but will also reduce the measurement precision by increasing the sensitivity to variations in other experimental variables.
5.3 Results obtained by these test methods are not strictly equivalent to those experienced in processing or handling conditions but may be used to rank materials for their volatility in such circumstances. Therefore, the volatility rates determined by these test methods should be considered as index values only.
5.4 The volatility rate may be used to estimate such quantifiable values as drying interval or the extent of volatile release from a process.
SCOPE
1.1 These test methods cover procedures for assessing the volatility of solids and liquids at given temperatures using thermogravimetry under prescribed experimental conditions. Results of these test methods are obtained as volatility rates expressed as mass per unit time. Rates ≥5 μg/min are achievable with these test methods.
1.2 Temperatures typical for these test methods are within the range from 25°C to 500°C. This temperature range may differ depending upon the instrumentation used.
1.3 These test methods are intended to provide a value for the volatility rate of a sample using a thermogravimetric analysis measurement on a single representative specimen. It is the responsibility of the user of these test methods to determine the need for and the number of repetitive measurements on fresh specimens necessary to satisfy end use requirements.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of these test methods to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The kinetic parameters combined with the general rate law and the reaction enthalpy can be used for the determination of thermal hazard using Practice E1231 (1).3
SCOPE
1.1 This test method covers the determination of the overall kinetic parameters for exothermic reactions using the Flynn/Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior can be described by the Arrhenius equation and the general rate law.
1.3 Limitations—There are cases where this technique is not applicable. Limitations may be indicated by curves departing from a straight line (see 11.2) or the isothermal aging test not closely agreeing with the results predicted by the calculated kinetic values. In particular, this test method is not applicable to reactions that are partially inhibited. The technique may not work with reactions that include simultaneous or consecutive reaction steps. This test method may not apply to materials that undergo phase transitions if the reaction rate is significant at the transition temperature.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.
5.2 This test method can be used for estimating lifetimes of materials, using Test Method E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 to 1300 K (nominally 100 to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 This test method is similar to ISO 11358-2 but differs in its mathematical treatment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the glass transition.
5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity.
5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events making it possible to determine the glass transition in the presence of interfering kinetic event.
5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance.
5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356), thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640).
SCOPE
1.1 These test methods describe the assignment of the glass transition temperature of materials using modulated temperature differential scanning calorimetry (MTDSC) over the temperature range from –120 to +600°C. The temperature range may be extended depending upon the instrumentation used.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There are no ISO equivalents to this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
5.1 These test methods are used to estimate the amount of volatile materials present in a material.
5.2 These test methods are useful for design purposes, service evaluation, regulatory statutes, manufacturing control, quality control, specification acceptance, development, and research.
5.3 The results obtained by these test methods may be equivalent to those obtained by other test methods and may be known by other terms in their respective fields. Other tests and terms encountered include loss-on-heating (see Footnote 5 and Test Methods D6, D2288, and E359); heating loss (see Test Method D1509); evaporative loss (see Test Method D2595); volatile organic carbon, moisture, or water (see Test Methods D2216 and D3175); volatility (see Test Method D4893); highly volatile matter (see Test Method E897); and volatile content (see Guide D2832).
SCOPE
1.1 These test methods describe a procedure for determining the amount of volatile matter of any kind that is driven off from a test specimen under a specific set of temperature and time conditions. These test methods determine only the mass of material lost, not its identity.
1.2 These test methods are applicable to a wide variety of solid or liquid materials, mixtures, or blends where the major component is stable at the test temperature.
Note 1: These test methods can be applied to the analysis of volatile organic compounds (VOC) content in metalworking fluids and direct contact lubricants subject to South Coast Air Quality Management District (SCAQMD) Rule 1144.
1.3 The applicable temperature range for these test methods are generally between ambient temperature and 1000°C.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 There is no ISO method equivalent to this test standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Oxidative induction time is a relative measure of the degree of oxidative stability of the material evaluated at the isothermal temperature of the test. The presence, quantity or effectiveness of antioxidants may be determined by this method. The OIT values thus obtained may be compared from one hydrocarbon to another or to a reference material to obtain relative oxidative stability information.
5.2 Typical uses include the oxidative stability of edible oils and fats (oxidative rancidity), lubricants, greases, and polyolefins.
SCOPE
1.1 These test methods describe the determination of the oxidative properties of hydrocarbons by differential scanning calorimetry or pressure differential scanning calorimetry and is applicable to hydrocarbons that oxidize exothermically in their analyzed form.
1.2 Test Method A—A differential scanning calorimeter (DSC) is used at ambient pressure, for example, about 100 kPa of oxygen.
1.3 Test Method B—A pressure DSC (PDSC) is used at high pressure, for example, 3.5 MPa (500 psig) oxygen.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 These test methods are related to ISO 11357–6 but is different in technical content. These test methods are related to CEC L-85–T but includes additional experimental conditions.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in 6.4 and 11.10.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.
5.2 This test method can be used for estimating lifetimes of materials, using Test Method E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and preexponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kineticsusing the Ozawa/Flynn/Wall isoconversional method (1, 2).2
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 to 1300K (nominally 100 to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 This test method is similar to ISO 11358-2 but differs in its mathematical treatment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
Frequently Asked Questions
E37.01 is a Technical Committee within ASTM International. It is named "Calorimetry and Mass Loss". This committee has published 155 standards.
E37.01 develops ASTM standards in the area of Information technology. Currently, there are 155 published standards from this technical committee.
ASTM is a standardization organization that develops and publishes standards to support industry, commerce, and regulatory requirements.
A Technical Committee (TC) in ASTM is a group of experts responsible for developing international standards in a specific technical area. TCs are composed of national member body delegates and work through consensus to create standards that meet global industry needs. Each TC may have subcommittees (SCs) and working groups (WGs) for specialized topics.