ASTM E1868-10(2015)

Standard Test Methods for Loss-On-Drying by Thermogravimetry

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.

General Information

• Status: Historical
• Publication Date: 30-Apr-2015
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1868 − 10 (Reapproved 2015)
Standard Test Methods for
Loss-On-Drying by Thermogravimetry
This standard is issued under the fixed designation E1868; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope (Moisture) Content of Soil and Rock by Mass
D2288 Test Method for Weight Loss of Plasticizers on
1.1 Thesetestmethodsdescribeaprocedurefordetermining
Heating (Withdrawn 2010)
theamountofvolatilematterofanykindthatisdrivenofffrom
D2595 Test Method for Evaporation Loss of Lubricating
a test specimen under a specific set of temperature and time
Greases Over Wide-Temperature Range
conditions. These test methods determine only the mass of
D2832 GuideforDeterminingVolatileandNonvolatileCon-
material lost, not its identity.
tent of Paint and Related Coatings
1.2 These test methods are applicable to a wide variety of
D3175 Test Method for Volatile Matter in the Analysis
solid or liquid materials, mixtures, or blends where the major
Sample of Coal and Coke
component is stable at the test temperature.
D4017 Test Method for Water in Paints and Paint Materials
NOTE 1—These test methods can be applied to the analysis of volatile
by Karl Fischer Method
organic compounds (VOC) content in metalworking fluids and direct
D4893 Test Method for Determination of Pitch Volatility
contactlubricantssubjecttoSouthCoastAirQualityManagementDistrict
E177 Practice for Use of the Terms Precision and Bias in
(SCAQMD) Rule 1144.
ASTM Test Methods
1.3 The applicable temperature range for these test methods
E359 Test Methods for Analysis of Soda Ash (Sodium
are generally between ambient temperature and 1000°C.
Carbonate)
1.4 The values stated in SI units are to be regarded as
E473 Terminology Relating to Thermal Analysis and Rhe-
standard. No other units of measurement are included in this
ology
standard.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.5 There is no ISO method equivalent to this test standard.
E897 TestMethodforVolatileMatterintheAnalysisSample
1.6 This standard does not purport to address all of the
of Refuse-Derived Fuel (Withdrawn 2011)
safety concerns, if any, associated with its use. It is the
E1142 Terminology Relating to Thermophysical Properties
responsibility of the user of this standard to establish appro-
E1582 Practice for Calibration of Temperature Scale for
priate safety and health practices and determine the applica-
Thermogravimetry
bility of regulatory limitations prior to use.
E1860 Test Method for Elapsed Time Calibration of Ther-
mal Analyzers
2. Referenced Documents
E2040 Test Method for Mass Scale Calibration of Thermo-
2.1 ASTM Standards:
gravimetric Analyzers
D6 Test Method for Loss on Heating of Oil and Asphaltic
2.2 SCAQMD Documents:
Compounds
Rule 1144 Metalworking Fluids and Direct-Contact Lubri-
D1475 Test Method For Density of Liquid Coatings, Inks,
cants
and Related Products
D1509 Test Methods for Carbon Black—Heating Loss
3. Terminology
D2216 Test Methods for Laboratory Determination of Water
3.1 Definitions:
3.1.1 Specific technical terms used in this test method are
These test methods are under the jurisdiction of ASTM Committee E37 on defined in Terminology E473 and Terminology E1142, includ-
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
ing thermogravimetry, thermogravimetric analyzer,
Calorimetry and Mass Loss.
repeatability, and reproducibility.
Current edition approved May 1, 2015. Published May 2015. Originally
approved in 1997. Last previous edition approved in 2010 as E1868 – 10. DOI:
10.1520/E1868-10R15.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer service at [e-mail]. For Annual Book of ASTM www.astm.org.
Standards volume information, refer to the standard’s Document Summary page on Available from South Coast Air Quality Management District (SCAQMD),
the ASTM website. 21865 Copley Drive, Diamond Bar, CA, 91765, http://aqmd.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1868 − 10 (2015)
4. Summary of Test Method 7. Apparatus
4.1 A specimen of known mass is heated at a constant 7.1 Thermogravimetric Analyzer, capable of continuously
recordingspecimenmassandtemperatureasafunctionoftime
temperature while its mass is continuously measured as a
function of time.At the end of a pre-determined time interval, consisting of:
orwhenthelossreachesapre-determinedrate,themasslossof 7.1.1 Electrobalance,withaminimumspecimencapacityof
thespecimen is recordedasapercentoftheoriginalmass.This 100 mg capable of continuously recording 10 µg or smaller
value is identified as the loss-on-drying (LOD) value. The masschanges.Performancemaybeverifiedinaccordancewith
LOD value is a function of both temperature and time. Test Method E2040.
Therefore these values must be identified and reported. A
7.1.2 Specimen Holders, that are inert to the specimen and
typical LOD value is reported as LOD = XX % (60 min at
of suitable structural shape and integrity to contain the 10 mg
120°C). The volatile content, V (g/L), or VOC content, VOC
test specimen used in these test methods. Specimen holders,
(g/L), may be calculated.
composed of platinum, aluminum, or quartz may be used, but
other holders may be considered.
NOTE 2—For SCAQMD Rule 1144 purposes, at the end of a pre-
determined time interval and specified temperature, the mass loss of the
NOTE3—ForSCAQMDRule 1144purposes,specimenholdersmustbe
specimen is recorded as a percent of the original mass. Additionally, the
shallow and composed of platinum.
density and water content of the sample are determined. These values are
7.1.3 Furnace, whose temperature can be controlled from
then used to calculate the VOC content.
25 to 1000°C, capable of a heating rate, at a minimum, of
5. Significance and Use 5°C/min and of maintaining a set temperature isothermally
within that range to 62°C.
5.1 These test methods are used to estimate the amount of
7.1.4 Temperature Sensor to provide an indication of the
volatile materials present in a material.
specimen or furnace temperature, or both, to 60.1°C.
5.2 These test methods are useful for design purposes,
NOTE 4—The temperature sensor shall be placed as close as practical to
service evaluation, regulatory statutes, manufacturing control,
the test specimen without disturbing weight measurements or as specified
quality control, specification acceptance, development, and
by the manufacturer. In addition, it must be located in exactly the same
research.
position during analytical determinations as used during calibration.
5.3 The results obtained by these test methods may be 7.1.5 Specimen Atmosphere Control System, capable of
supplying inert dry gas (usually purified grade nitrogen) with
equivalent to those obtained by other test methods and may be
known by other terms in their respective fields. Other tests and an operator selectable flow rate of 50 to 100 mL⁄min to within
65 mL⁄min.
terms encountered include loss-on-heating (see Footnote and
Test Methods D6, D2288, and E359); heating loss (see Test
NOTE 5—For SCAQMD Rule 1144 purposes, use purified grade nitro-
Method D1509); evaporative loss (see Test Method D2595);
gen for both the sample purge flow and balance protection flow.
volatile organic carbon, moisture, or water (see Test Methods
7.1.6 Measurement System, to continuously record speci-
D2216andD3175);volatility(seeTestMethodD4893);highly
men temperature to within 60.1°C over the range from 25 to
volatile matter (see Test Method E897); and volatile content
1000°C.
(see Guide D2832).
7.1.7 Timer, capable of continuously recording elapsed time
up to 20 h to within 6 0.1 min or 61 %, whichever is greater.
6. Interferences
Performance may be verified in accordance with Test Method
6.1 Becausethespecimensizeisusuallysmall,caremustbe
E1860.
taken to ensure that each specimen is representative of the
7.1.8 Controller, capable of executing a temperature pro-
sample as a whole.
gram by operating the furnace from 25 to 1000°C at a
minimum rate of 5°C/min to within 60.1°C/min and of
6.2 This test procedure measures total mass loss under
maintaining a set temperature isothermally within the range of
specific experimental conditions. If more than one volatile
62°C.
component is present, the results will reflect the total of all
7.1.9 Data Collection Device,provideameansofacquiring,
those volatile components present.
storing, and displaying measured or calculated signals, or both.
6.3 If the test temperature is set too high, the resultant
The minimum output signals required for thermogravimetric
weight loss may include some decomposition of the matrix
analysis (TGA) are mass, temperature, and time.
material.
7.1.10 While not required, it is convenient to have a data
analysis device that will continuously perform and display the
6.4 When calculating VOC content for SCAQMD
following calculation:
Rule 1144 purposes, it may be necessary to measure and
correct for water content. Refer to Test Method D4017 to 7.1.10.1 Specimen mass as a percent of the initial mass.
determine the water content of the specimen.
7.1.10.2 Specimen mass rate of change (in mass %⁄min)
capable of detecting 0.01 %⁄min.
7.1.11 While not required, it is convenient to have an
experiment control device capable of terminating the experi-
Formulary Vol XVII is available from U.S. Pharmacopeia (USP), 12601
Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org. ment under the following conditions:
E1868 − 10 (2015)
7.1.11.1 When an operator selected period of time at an 11.1 Obtain a suitable baseline correction.
isothermal temperature condition has elapsed, and
11.2 Set the furnace and flow parameters.
7.1.11.2 When an operator selected rate of mass loss is
NOTE 10—For SCAQMD Rule 1144 purposes, the total flow must be
achieved.
50 mL⁄min, divided (balance protection flow:sample purge flow) either
7.2 Gas Exhaust System capable of removing from the
10:40 mL/min or 20:30 mL/min.
laboratory the potentially noxious purge gas effluent of the
11.3 Coolthespecimentestareaoftheapparatustoambient
system above.
temperature. For the purpose of this test, ambient temperature
7.3 Inert Gas—Purified grade nitrogen. is 35°C or lower.
7.4 Micropipettes or Syringes, for liquids, capable of dis-
NOTE 11—Cooling of the specimen test area to 25°C following an
experiment is time consuming on some apparatus. To improve
pensing up to 15 6 1 µL.
productivity, it is possible with some test samples to initiate the experi-
8. Hazards ment at a somewhat higher temperature. This must be done with caution
since volatility is a function of temperature. For highly volatile materials,
8.1 Toxic or corrosive effluent, or both, may be released
appreciableportionsofthetestspecimenmassmaybelostinexperimental
when heating some materials and could be harmful to person-
set up, if initiated at too high of a temperature.
NOTE 12—For SCAQMD Rule 1144 purposes, initial temperature is
nel and to apparatus.
25 6 2°C.
9. Sampling
11.4 With the apparatus closed in the normal operating
9.1 Samples are usually analyzed on “as received” basis.
position, tare the balance so that the empty sample pan
Should some thermal or mechanical treatment (such as grind-
indicates zero mass.
ing or sieving) be applied to the sample prior to analysis, it
11.5 Open the apparatus to expose the specimen holder.
shall be indicated in the report. Grinding may release volatiles
11.6 Carefully place 10 6 1 mg of the test specimen on the
due to the heating generated by grinding process.
specimen holder. Other specimen sizes may be used but must
9.2 Since small test specimens are used, they must be
be indicated in the report.
homogeneous and representative of the sample. The mixing or
NOTE 13—Care should be taken to ensure that the sample is free of air
stirring of samples prior to analysis is recommended whenever
bubbles.
possible. NOTE 14—For SCAQMD Rule 1144 purposes, specimen size is
10 6 1 µL, autosamplers are not to be used and the specimen must be
9.3 If experiments are to be initiated at room temperature,
distributed evenly over the bottom of the specimen holder.
equilibrate samples in their sealed containers to room tempera-
11.7 Close the apparatus and record the initial mass as m.If
i
ture prior to testing.
the apparatus has provisions for direct recording of mass
NOTE 6—For SCAQMD Rule 1144 purposes, samples containing solid
percent, adjust it to read 100 %.
particles should be filtered prior to analysis.
NOTE 15—Should the test specimen have appreciable volatility at
10. Calibration
ambient temperature, it may lose a significant amount of mass as it is
placedintothetestposition.Insuchcases,careshouldbetakentoperform
10.1 Calibrate the temperature signal from the apparatus
11.6 and 11.7 as quickly as is practical.
according to Practice E1582 using a heating rate of 1°C/min
11.8 Heatthetestspecimenat5°C/mintotheisothermaltest
and a transition temperature close to the isothermal test
temperature,whilerecordingspecimenmass(ormasspercent),
temperature used in this procedure.
temperatureandelapsedtime.Otherheatingratesmaybeused,
10.2 Calibrate the mass signal from the apparatus according
but must be indicated in the report.
to Test Method E2040.
NOTE16—Selectionoftheoptimumoperatingparametersofisothermal
NOTE 7—Regular analysis of performance standards (materials of
test temperature and test time (t) is dependent on the class of materials
t
known mass loss characteristics) where available, serves as a check on
being tested. The technique of response surface methodology (RSM) may
7,8
instrument status, operator efficiency, etc., and provides for a comparison
be useful in predicting optimum operating parameters. Some common
of results from different laboratories. Verify mass measurement confor-
experimental conditions are presented in Tables 1 and 2.
mity to better than 1 %. Verify time measurement conformity to better
NOTE17—ForSCAQMDRule 1144purposes,heatingrateis25°C/min
than 1 %.
and isothermal test temperature is 81°C.
10.3 Calibrate the time signal from the apparatus according
11.9 Once the isothermal test temperature is reached, it is
to Test Method E1860.
held there for the remainder of the experiment. The time from
start to the isothermal portion of the experiment is taken as t.
i
NOTE 8—For SCAQMD Rule 1144
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1868 − 10 E1868 − 10 (Reapproved 2015)
Standard Test MethodMethods for
Loss-On-Drying by Thermogravimetry
This standard is issued under the fixed designation E1868; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 ThisThese test method describesmethods 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. ThisThese test method
determinesmethods determine only the mass of material lost, not its identity.
1.2 ThisThese test method ismethods 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—ThisThese test methodmethods 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 thisthese test method ismethods 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.
2. Referenced Documents
2.1 ASTM Standards:
D6 Test Method for Loss on Heating of Oil and Asphaltic Compounds
D1475 Test Method For Density of Liquid Coatings, Inks, and Related Products
D1509 Test Methods for Carbon Black—Heating Loss
D2216 Test Methods for Laboratory Determination of Water (Moisture) Content of Soil and Rock by Mass
D2288 Test Method for Weight Loss of Plasticizers on Heating (Withdrawn 2010)
D2595 Test Method for Evaporation Loss of Lubricating Greases Over Wide-Temperature Range
D2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings
D3175 Test Method for Volatile Matter in the Analysis Sample of Coal and Coke
D4017 Test Method for Water in Paints and Paint Materials by Karl Fischer Method
D4893 Test Method for Determination of Pitch Volatility
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E359 Test Methods for Analysis of Soda Ash (Sodium Carbonate)
E473 Terminology Relating to Thermal Analysis and Rheology
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E897 Test Method for Volatile Matter in the Analysis Sample of Refuse-Derived Fuel (Withdrawn 2011)
E1142 Terminology Relating to Thermophysical Properties
E1582 Practice for Calibration of Temperature Scale for Thermogravimetry
E1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
ThisThese test method ismethods are under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01
on Calorimetry and Mass Loss.
Current edition approved July 1, 2010May 1, 2015. Published August 2010May 2015. Originally approved in 1997. Last previous edition approved in 20092010 as
E1868 – 09.E1868 – 10. DOI: 10.1520/E1868-10.10.1520/E1868-10R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1868 − 10 (2015)
E2040 Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
2.2 SCAQMD Documents:
Rule 1144 Metalworking Fluids and Direct-Contact Lubricants
3. Terminology
3.1 Definitions:
3.1.1 Specific technical terms used in this test method are defined in Terminology E473 and Terminology E1142,
includeincluding thermogravimetry, thermogravimetric analyzer, repeatability, and reproducibility.
4. Summary of Test Method
4.1 A specimen of known mass is heated at a constant temperature while its mass is continuously measured as a function of time.
At the end of a pre-determined time interval, or when the loss reaches a pre-determined rate, the mass loss of the specimen is
recorded as a percent of the original mass. This value is identified as the loss-on-drying (LOD) value. The LOD value is a function
of both temperature and time. Therefore these values must be identified and reported. A typical LOD value is reported as LOD =
XX % (60 min at 120°C). The volatile content, V (g/L), or VOC content, VOC (g/L), may be calculated.
NOTE 2—For SCAQMD Rule 1144 purposes, at the end of a pre-determined time interval and specified temperature, the mass loss of the specimen
is recorded as a percent of the original mass. Additionally, the density and water content of the sample are determined. These values are then used to
calculate the VOC content.
5. Significance and Use
5.1 ThisThese test method ismethods are used to estimate the amount of volatile materials present in a material.
5.2 ThisThese test method ismethods are useful for design purposes, service evaluation, regulatory statutes, manufacturing
control, quality control, specification acceptance, development, and research.
5.3 The results obtained by thisthese test methodmethods 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 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).
6. Interferences
6.1 Because the specimen size is usually small, care must be taken to ensure that each specimen is representative of the sample
as a whole.
6.2 This test procedure measures total mass loss under specific experimental conditions. If more than one volatile component
is present, the results will reflect the total of all those volatile components present.
6.3 If the test temperature is set too high, the resultant weight loss may include some decomposition of the matrix material.
6.4 When calculating VOC content for SCAQMD Rule 1144 purposes, it may be necessary to measure and correct for water
content. Refer to Test Method D4017 to determine the water content of the specimen.
7. Apparatus
7.1 Thermogravimetric Analyzer, capable of continuously recording specimen mass and temperature as a function of time
consisting of:
7.1.1 Electrobalance, with a minimum specimen capacity of 100 mg capable of continuously recording 10 μg or smaller mass
changes. Performance may be verified in accordance with Test Method E2040.
7.1.2 Specimen Holders, that are inert to the specimen and of suitable structural shape and integrity to contain the 10 mg test
specimen used in thisthese test method.methods. Specimen holders, composed of platinum, aluminum, or quartz may be used, but
other holders may be considered.
NOTE 3—For SCAQMD Rule 1144 purposes, specimen holders must be shallow and composed of platinum.
7.1.3 Furnace, whose temperature can be controlled from 25 to 1000°C, capable of a heating rate, at a minimum, of 5°C/min
and of maintaining a set temperature isothermally within that range to 62°C.
7.1.4 Temperature Sensor to provide an indication of the specimen or furnace temperature, or both, to 60.1°C.
NOTE 4—The temperature sensor shall be placed as close as practical to the test specimen without disturbing weight measurements or as specified by
the manufacturer. In addition, it must be located in exactly the same position during analytical determinations as used during calibration.
Available from South Coast Air Quality Management District (SCAQMD), 21865 Copley Drive, Diamond Bar, CA, 91765, http://aqmd.gov.
Formulary Vol XVII is available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org.
E1868 − 10 (2015)
7.1.5 Specimen Atmosphere Control System, capable of supplying inert dry gas (usually purified grade nitrogen) with an
operator selectable flow rate of 50 to 100 mL ⁄min to within 65 mL ⁄min.
NOTE 5—For SCAQMD Rule 1144 purposes, use purified grade nitrogen for both the sample purge flow and balance protection flow.
7.1.6 Measurement System, to continuously record specimen temperature to within 60.1°C over the range from 25 to 1000°C.
7.1.7 Timer, capable of continuously recording elapsed time up to 20 h to within 6 0.1 min or 61 %, whichever is greater.
Performance may be verified in accordance with Test Method E1860.
7.1.8 Controller, capable of executing a temperature program by operating the furnace from 25 to 1000°C at a minimum rate
of 5°C/min to within 60.1°C/min and of maintaining a set temperature isothermally within the range of 62°C.
7.1.9 Data Collection Device, provide a means of acquiring, storing, and displaying measured or calculated signals, or both. The
minimum output signals required for thermogravimetric analysis (TGA) are mass, temperature, and time.
7.1.10 While not required, it is convenient to have a data analysis device that will continuously perform and display the
following calculation:
7.1.10.1 Specimen mass as a percent of the initial mass.
7.1.10.2 Specimen mass rate of change (in mass % ⁄min) capable of detecting 0.01 % ⁄min.
7.1.11 While not required, it is convenient to have an experiment control device capable of terminating the experiment under
the following conditions:
7.1.11.1 When an operator selected period of time at an isothermal temperature condition has elapsed, and
7.1.11.2 When an operator selected rate of mass loss is achieved.
7.2 Gas Exhaust System capable of removing from the laboratory the potentially noxious purge gas effluent of the system above.
7.3 Inert Gas—Purified grade nitrogen.
7.4 Micropipettes or Syringes, for liquids, capable of dispensing up to 15 6 1 μL.
8. Hazards
8.1 Toxic or corrosive effluent, or both, may be released when heating some materials and could be harmful to personnel and
to apparatus.
9. Sampling
9.1 Samples are usually analyzed on “as received” basis. Should some thermal or mechanical treatment (such as grinding or
sieving) be applied to the sample prior to analysis, it shall be indicated in the report. Grinding may release volatiles due to the
heating generated by grinding process.
9.2 Since small test specimens are used, they must be homogeneous and representative of the sample. The mixing or stirring
of samples prior to analysis is recommended whenever possible.
9.3 If experiments are to be initiated at room temperature, equilibrate samples in their sealed containers to room temperature
prior to testing.
NOTE 6—For SCAQMD Rule 1144 purposes, samples containing solid particles should be filtered prior to analysis.
10. Calibration
10.1 Calibrate the temperature signal from the apparatus according to Practice E1582 using a heating rate of 1°C/min and a
transition temperature close to the isothermal test temperature used in this procedure.
10.2 Calibrate the mass signal from the apparatus according to Test Method E2040.
NOTE 7—Regular analysis of performance standards (materials of known mass loss characteristics) where available, serves as a check on instrument
status, operator efficiency, etc., and provides for a comparison of results from different laboratories. Verify mass measurement conformity to better than
1 %. Verify time measurement conformity to better than 1 %.
10.3 Calibrate the time signal from the apparatus according to Test Method E1860.
NOTE 8—For SCAQMD Rule 1144 purposes, calibrate the mass signal every week, the temperature signal every three months, and the time signal every
six months.
11. Procedure
NOTE 9—For SCAQMD Rule 1144 purposes, additional proceedures may be required by the agency.
11.1 Obtain a suitable baseline correction.
11.2 Set the furnace and flow parameters.
Performance Standards for low (2 %), medium (50 %), and high (99 %) LOD values are available from several suppliers. Contact ASTM International for list of suppliers.
E1868 − 10 (2015)
NOTE 10—For SCAQMD Rule 1144 purposes, the total flow must be 50 mL ⁄min, divided (balance protection flow:sample purge flow) either 10:40
mL/min or 20:30 mL/min.
11.3 Cool the specimen test area of the apparatus to ambient temperature. For the purpose of this test, ambient temperature is
35°C or lower.
NOTE 11—Cooling of the specimen test area to 25°C following an experiment is time consuming on some apparatus. To improve productivity, it is
possible with some test samples to initiate the experiment at a somewhat higher temperature. This must be done with caution since volatility is a function
of temperature. For highly volatile materials, appreciable portions of the test specimen mass may be lost in experimental set up, if initiated at too high
of a temperature.
NOTE 12—For SCAQMD Rule 1144 purposes, initial temperature is 25 6 2°C.
11.4 With the apparatus closed in the normal operating position, tare the balance so that the empty sample pan indicates zero
mass.
11.5 Open the apparatus to expose the specimen holder.
11.6 Carefully place 10 6 1 mg of the test specimen on the specimen holder. Other specimen sizes may be used but must be
indicated in the report.
NOTE 13—Care should be taken to ensure that the sample is free of air bubbles.
NOTE 14—For SCAQMD Rule 1144 purposes, specimen size is 10 6 1 μL, autosamplers are not to be used and the specimen must be distributed evenly
over the bottom of the specimen holder.
11.7 Close the apparatus and record the initial mass as m . If the apparatus has provisions for direct recording of mass percent,
i
a
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