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ASTM B808-97

(Test Method)

Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal Microbalances

Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal Microbalances

SCOPE
1.1 This test method monitors the reactivity of a gaseous test environment in which metal surfaces (that is, electrical contacts) and other materials subject to pollutant gas attack, undergo accelerated atmospheric corrosion testing. This test method is applicable to adherent corrosion films whose total corrosion film thickness ranges from a few atomic monolayers to approximately a micrometer.
1.2 The test method provides a dynamic, continuous, in situ, procedure for monitoring the corrosion rate in corrosion chambers; the uniformity of corrosion chambers; and the corrosion rate on different surfaces. Response time of the order of seconds is possible.
1.3 With the proper samples, the quartz crystal microbalance (QCM) test method can also be used to monitor the weight loss from a surface due to the desorption of surface species (that is, reduction of an oxide in a reducing atmosphere). (Alternative names for QCM are quartz crystal oscillator, piezoelectric crystal oscillator, or thin film evaporation monitor.)
1.4 This test method is not sufficient to specify the corrosion process which may be occurring in a chamber, since a variety of pollutant gases and environments may cause similar weight gains.
1.5 This test method is generally not applicable to test environments where solid or liquid particles are deposited on the surface of the quartz crystal.
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.  
1.7 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.

General Information

Status
Historical
Publication Date
09-Mar-1997
ICS
77.060 - Corrosion of metals
Technical Committee
B02 - Nonferrous Metals and Alloys
Drafting Committee
B02.11 - Electrical Contact Test Methods
Current Stage
Ref Project

Relations

Replaced By
ASTM B808-97(2003) - Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal Microbalances
Effective Date
01-Nov-2003
Referred By
ASTM B845-97(2018) - Standard Guide for Mixed Flowing Gas (MFG) Tests for Electrical Contacts
Effective Date
10-Mar-1997
Referred By
ASTM B826-09(2020) - Standard Test Method for Monitoring Atmospheric Corrosion Tests by Electrical Resistance Probes
Effective Date
10-Mar-1997
Referred By
ASTM B827-05(2020) - Standard Practice for Conducting Mixed Flowing Gas (MFG) Environmental Tests
Effective Date
10-Mar-1997
Referred By
ASTM B825-19 - Standard Test Method for Coulometric Reduction of Surface Films on Metallic Test Samples
Effective Date
10-Mar-1997

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ASTM B808-97 - Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal MicrobalancesASTM B808-97 - Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal Microbalances
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ASTM B808-97 - Standard Test Method for Monitoring of Atmospheric Corrosion Chambers by Quartz Crystal Microbalances
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: B 808 – 97
Standard Test Method for
Monitoring of Atmospheric Corrosion Chambers by Quartz
Crystal Microbalances
This standard is issued under the fixed designation B 808; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method monitors the reactivity of a gaseous 2.1 ASTM Standards:
test environment in which metal surfaces (for example, elec- B 810 Test Method for Calibration of Atmospheric Corro-
trical contacts, assembled printed wiring boards, and so forth) sion Test Chambers by Change in Mass of Copper Cou-
and other materials subject to pollutant gas attack undergo pons
accelerated atmospheric corrosion testing. This test method is
3. Summary of Test Method
applicable to adherent corrosion films whose total corrosion
3.1 A single crystal of quartz has various natural resonant
film thickness ranges from a few atomic monolayers to
approximately a micrometre. frequencies depending on the crystal’s size and shape. The
decrease in natural frequency is linearly proportional to the
1.2 The test method provides a dynamic, continuous, in-
situ, procedure for monitoring the corrosion rate in corrosion crystal mass and the mass of well-bonded surface films. For
crystals with reactive metal films on the surface (usually
chambers; the uniformity of corrosion chambers; and the
corrosion rate on different surfaces. Response time in the order driving electrodes), the mass of the crystal/metal film increases
as the metal oxidizes or forms other compounds with gases
of seconds is possible.
3,4
1.3 With the proper samples, the quartz crystal microbal- adsorbed from the atmosphere. Thus, by measuring the rate
of resonant frequency change, a rate of corrosion is measured.
ance (QCM) test method can also be used to monitor the
weight loss from a surface as a result of the desorption of Non-adherent corrosion films, particles, and droplets yield
ambiguous results. A review of theory and applications is given
surface species (that is, reduction of an oxide in a reducing
atmosphere). (Alternative names for QCM are quartz crystal in Lu and Czanderna.
3.2 The chamber environmental uniformity and corrosion
oscillator, piezoelectric crystal oscillator, or thin-film evapora-
tion monitor.) rate can be measured by placing matching quartz crystals with
matching reactive metal films at various locations in the
1.4 This test method is not sufficient to specify the corrosion
process that may be occurring in a chamber, since a variety of chamber. If the chamber and corrosion rate have been stan-
dardized, the corrosion rate on various surface materials that
pollutant gases and environments may cause similar weight
gains. have been deposited on the quartz crystal can be determined.
1.5 This test method is generally not applicable to test
4. Significance and Use
environments in which solid or liquid particles are deposited on
4.1 Corrosion film growth with thicknesses varying from a
the surface of the quartz crystal.
monolayer of atoms up to 1 μm can readily be measured on a
1.6 This standard does not purport to address all of the
continuous, real-time, in-situ, basis with QCMs.
safety concerns, if any, associated with its use. It is the
4.2 The test results obtained for this test method are
responsibility of the user of this standard to establish appro-
influenced by various factors, including geometrical effects,
priate safety and health practices and determine the applica-
temperature, humidity, film thickness, film materials, electrode
bility of regulatory limitations prior to use.
conditions, gases in the corrosion chamber, and so forth.
1.7 The values stated in SI units are to be regarded as the
standard. The values in parentheses are for information only.
Annual Book of ASTM Standards, Vol 03.04.
King, W. H. Jr., Analytical Chemistry, Vol 36, 1964, p. 173.
1 4
This test method is under the jurisdiction of ASTM Committee B-2 on Karmarkar, K. H. and Guilbaut, G. G. Analytical Chemistry Acta, Vol 75, 1975,
Nonferrous Metals and Alloys and is the direct responsibility of Subcommittee p. 111.
B02.11 on Electrical Contact Test Methods. Lu, C. and Czanderna, A. W. Eds., Applications of Piezoelectric Quartz Crystal
Current edition approved March 10, 1997. Published January 1998. Microbalances, Elsevier, c1984.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
B808–97
Calibration of coated crystals and instrumentation and repro- the fragility of the metal electrode there should be multiple
ducible crystal operating conditions are necessary for consis- (three or more), spring-loaded contacts between the crystal and
tent results. electronics.
6.3 After metallization of the crystals, they should be stored
5. Apparatus
in desiccators. After two years storage or if the metallization
shows discoloration or staining, the crystals shall be discarded.
5.1 Apparatus can be a simple series circuit of crystal (with
Crystal surfaces should not be chemically or mechanically
electrodes and sensing film), oscillator (typically 6 MHz) and
cleaned before use in the corrosion chamber. They should be
frequency counter (610-Hz accuracy and stability), as sche-
blown clean with inert compressed gas. Chilling and conden-
matically shown in Fig. 1.
sation on the surface, as can occur with the use of pressurized
fluorocarbons, shall be avoided. Care shall be exercised so that
the crystals are only handled by clean tweezers or tongs and
never touched by hands.
7. Calibration
7.1 QCMs and its electronics shall be calibrated initially in
a given corrosion system and thereafter on an annual basis.
FIG. 1 Schematic of QCM and Related Electronics Calibration shall be performed with the same shape and size of
crystal holder to be used during operation. Recalibration shall
be performed if the crystal holder geometry is changed.
5.2 Commercial, Thin-Film Monitors, incorporating those
Calibration can be done by comparison to a standard such as
functions that read out thicknesses or weight gain are also actual gravimetric weighing on a microbalance (62 μg). Use a
available and acceptable after they have been calibrated.
sample of the same material as the sensing film with a
5.3 Balance, with an accuracy of 62 μg is needed for
minimum area of 5 cm and a thickness of 0.1 to 0.6 mm (see
calibration procedures.
Test Method B 810). Foil surface roughness should be within
5.4 Recording Devices or Computers are needed for real-
620 % of the QCM sensing film roughness. The procedure for
time, continuous measurements.
the generation (that is, evaporation) and cleaning of the
gravimetric sample should be the same as used for the sensing
6. Materials
films. The age and storage of the gravimetric sample should be
comparable to the age of the QCM sensing film. Allow the foil
6.1 Crystals shall be of the AT cut variety with a resonant
to equilibrate with the microbalance atmosphere for 0.5 h, then
frequency in the MHz range and matched to the frequency
weigh the sample with 62-μg accuracy before exposure.
measuring apparatus used. Quartz c
...

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Standard Practice for Determining the Susceptibility of Stainless Steels and Related Nickel-Chromium-Iron Alloys to Stress-Corrosion Cracking in Polythionic Acids

SIGNIFICANCE AND USE
4.1 Polythionic acids are chemically described as H2SxO6, where x is usually 3, 4, or 5 (1)3 though can be more than 50 (2). These acid environments provide a way of evaluating the resistance of stainless steels and related alloys to intergranular stress corrosion cracking. Failure is accelerated by the presence of increasing amounts of intergranular precipitate. Results for the polythionic acid test have not been correlated exactly with those of intergranular corrosion tests (Test Methods G28). Also, this test may not be relevant to stress corrosion cracking in chlorides or caustic environments.  
4.2 The polythionic acid environment may produce areas of shallow intergranular attack in addition to the more localized and deeper cracking mode of attack. Examination of failed specimens is necessary to confirm that failure occurred by cracking rather than mechanical failure of reduced sections.
SCOPE
1.1 This practice covers procedures for preparing and conducting the polythionic acid test at room temperature, 22 °C to 25 °C (72 °F to 77 °F), to determine the relative susceptibility of stainless steels or other related materials (nickel-chromium-iron alloys) to intergranular stress corrosion cracking.  
1.2 This practice can be used to evaluate stainless steels or other materials in the “as received” condition or after being subjected to high-temperature service, 482 °C to 815 °C (900 °F to 1500 °F), for prolonged periods of time.  
1.3 This practice can be applied to wrought products, castings, and weld metal of stainless steels or other related materials to be used in environments containing sulfur or sulfides. Other materials capable of being sensitized can also be tested in accordance with this test.  
1.4 This practice may be used with a variety of stress corrosion test specimens, surface finishes, and methods of applying stress.  
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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. For more specific precautionary statements, see Section 7.  
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.

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