0% found this document useful (0 votes)
136 views9 pages

Astm B827

STANDARD PRACTICE FOR CONDUCTIVE MIXED FLOWING GAS

Uploaded by

controldocs
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
136 views9 pages

Astm B827

STANDARD PRACTICE FOR CONDUCTIVE MIXED FLOWING GAS

Uploaded by

controldocs
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 9

Designation: B 827 – 97 (Reapproved 2003)

Standard Practice for


Conducting Mixed Flowing Gas (MFG) Environmental Tests1
This standard is issued under the fixed designation B 827; 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 B 825 Test Method for Coulometric Reduction of Surface


1.1 This practice provides procedures for conducting envi- Films on Metallic Test Samples2
ronmental tests involving exposures to controlled quantities of B 826 Test Method for Monitoring Atmospheric Corrosion
corrosive gas mixtures. Tests by Electrical Resistance Probes2
1.2 This practice provides for the required equipment and B 845 Guide for Mixed Flowing Gas (MFG) Tests for
methods for gas, temperature, and humidity control which Electrical Contacts2
enable tests to be conducted in a reproducible manner. Repro- D 1193 Specification for Reagent Water4
ducibility is measured through the use of control coupons D 1607 Test Method for Nitrogen Dioxide Content of the
whose corrosion films are evaluated by mass gain, coulometry, Atmosphere (Griess-Saltzman Reaction)5
or by various electron and X-ray beam analysis techniques. D 2912 Test Method for Oxidant Content of the Atmo-
Reproducibility can also be measured by in situ corrosion rate sphere (Neutral KI)6
monitors using electrical resistance or mass/frequency change D 2914 Test Methods for Sulfur Dioxide Content of the
methods. Atmosphere (West-Gaeke Method)5
1.3 The values stated in SI units are to be regarded as the D 3449 Test Method for Sulfur Dioxide in Workplace At-
standard. mospheres (Barium Perchlorate Method)6
1.4 This standard does not purport to address all of the D 3464 Test Method for Average Velocity in a Duct Using a
safety concerns, if any, associated with its use. It is the Thermal Anemometer5
responsibility of the user of this standard to become familiar D 3609 Practice for Calibration Techniques Using Perme-
with all hazards including those identified in the appropriate ation Tubes5
Material Safety Data Sheet for this product/material as pro- D 3824 Test Methods for Continuous Measurement of Ox-
vided by the manufacturer, to establish appropriate safety and ides of Nitrogen in the Ambient or Workplace Atmosphere
health practices, and determine the applicability of regulatory by the Chemiluminescent Method5
limitations prior to use. See 5.1.2.4. D 4230 Test Method of Measuring Humidity With Cooled-
Surface Condensation (Dew-Point) Hygrometer5
2. Referenced Documents E 902 Practice for Checking the Operating Characteristics
2.1 ASTM Standards: of X-Ray Photoelectron Spectrometers7
B 542 Terminology Relating to Electrical Contacts and G 91 Practice for Monitoring Atmospheric SO2 Using Sul-
Their Use2 fation Plate Technique8
B 765 Guide for Selection of Porosity Tests for Electrode-
3. Terminology
posits and Related Metallic Coatings3
B 808 Test Method for Monitoring of Atmospheric Corro- 3.1 Definitions relating to electrical contacts are in accor-
sion Chambers by Quartz Crystal Microbalances2 dance with Terminology B 542.
B 810 Test Method for Calibration of Atmospheric Corro- 4. Significance and Use
sion Test Chambers by Change in Mass of Copper Cou-
pons2 4.1 Mixed flowing gas (MFG) tests are used to simulate or
amplify exposure to environmental conditions which electrical
1
This practice is under the jurisdiction of ASTM Committee B02 on Nonferrous
Metals and Alloys and is the direct responsibility of Subcommittee B02.11 on
4
Electrical Contact Test Methods. Annual Book of ASTM Standards, Vol 11.01.
5
Current edition approved June 10, 2003. Published July 2003. Originally Annual Book of ASTM Standards, Vol 11.03.
6
approved in 1992. Last previous edition approved in 1997 as B 827 - 97. Discontinued; see 1990 Annual Book of ASTM Standards, Vol 11.03.
2 7
Annual Book of ASTM Standards, Vol 02.04. Annual Book of ASTM Standards, Vol 03.06.
3 8
Annual Book of ASTM Standards, Vol 02.05. Annual Book of ASTM Standards, Vol 03.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
B 827 – 97 (2003)
contacts or connectors can be expected to experience in various ture to a maximum tolerance of 61°C with a preferred
application environments (1, 2).9 tolerance held to 60.5°C within the usable chamber working
4.2 Test samples which have been exposed to MFG tests space accordance with 7.3, with a means to introduce and
have ranged from bare metal surfaces, to electrical connectors, exhaust gases from the chamber.
and to complete assemblies. 5.1.1.2 The chamber isolates the reactive gases from the
4.3 The specific test conditions are usually chosen so as to external environment. Chamber materials that are not low-
simulate, in the test laboratory, the effects of certain represen- absorbing can affect test conditions by absorbing or emitting
tative field environments or environmental severity levels on reactive gases, leading to control and reproducibility problems.
standard metallic surfaces, such as copper and silver coupons The chamber construction shall be such that the leak rate is less
or porous gold platings (1, 2). than 3 % of the volume exchange rate.
4.4 Because MFG tests are simulations, both the test con- 5.1.1.3 The chamber shall have provision for maintaining
ditions and the degradation reactions (chemical reaction rate, uniformity of the average gas flow velocity within 620 % of a
composition of reaction products, etc.) may not always re- specified value or of the chamber average when the chamber is
semble those found in the service environment of the product empty. For chambers with a dimension of more than 0.5 m,
being tested in the MFG test. A guide to the selection of measurement points shall be in accordance with Test Method
simulation conditions suitable for a variety of environments is B 810. For chambers with all dimensions of less than 0.5 m, a
found in Guide B 845. minimum of five points shall be measured at locations in the
4.5 The MFG exposures are generally used in conjunction plane of sample exposure (perpendicular to the expected flow
with procedures which evaluate contact or connector electrical direction) that are equidistant from each other and the walls of
performance such as measurement of electrical contact resis- the chamber. After all five or more data values are recorded, all
tance before and after MFG exposure. measurements shall be repeated a second time. After the two
4.6 The MFG tests are useful for connector systems whose sets of measurements are recorded, a third complete set shall be
contact surfaces are plated or clad with gold or other precious recorded. The arithmetic average of the 15 or more measure-
metal finishes. For such surfaces, environmentally produced ments shall be the chamber average. See 7.5 and 7.6.8. If a hot
failures are often due to high resistance or intermittences wire anemometer is used for gas velocity measurements, it
caused by the formation of insulating contamination in the shall be made in accordance with Test Method D 3464, with
contact region. This contamination, in the form of films and the exception that sample sites shall be in accordance with Test
hard particles, is generally the result of pore corrosion and Method B 810.
corrosion product migration or tarnish creepage from pores in 5.1.1.4 A sample access port is desirable. This should be
the precious metal coating and from unplated base metal designed such that control coupons can be removed or replaced
boundaries, if present. without interrupting the flow of gases. Corrosion test chamber
4.7 The MFG exposures can be used to evaluate novel corrosion rates have been shown to be a function of the
electrical contact metallization for susceptibility to degradation presence or absence of light (3, 4). Provision for controlling the
due to environmental exposure to the test corrosive gases. test illumination level in accordance with a test specification
4.8 The MFG exposures can be used to evaluate the shall be made.
shielding capability of connector housings which may act as a
5.1.1.5 Examples of test chamber systems are diagrammed
barrier to the ingress of corrosive gases.
in Figs. 1-3. They are not to be considered exclusive examples.
4.9 The MFG exposures can be used to evaluate the
susceptibility of other connector materials such as plastic 5.1.2 Gas Supply System:
housings to degradation from the test corrosive gases. 5.1.2.1 Description and Requirements—The gas supply sys-
4.10 The MFG tests are not normally used as porosity tests. tem consists of five main parts: a source of clean, dry, filtered
For a guide to porosity testing, see Guide B 765. air; a humidity source; corrosive gas source(s); gas delivery
4.11 The MFG tests are generally not applicable where the system; and corrosive gas concentration monitoring system(s).
failure mechanism is other than pollutant gas corrosion such as Total supply capacity must be such as to meet requirements for
in tin-coated separable contacts. control of gas concentrations. The minimum number of volume
changes is determined by the requirement that the concentra-
5. Apparatus tion of corrosive gases be maintained within 615 % between
5.1 Apparatus required to conduct MFG tests are divided gas inlet and outlet. This is verified by measurement of the gas
into four major categories, corrosion test chamber, gas supply concentrations near the gas inlet upstream of the usable
system, chamber monitoring system, and chamber operating chamber working volume and comparing with gas concentra-
system. tions measured downstream of the usable chamber working
5.1.1 Corrosion Test Chamber: volume just prior to the chamber exhaust; these values shall be
5.1.1.1 The chamber shall consist of an enclosure made of within 615 % (see 7.6). Alternative methods of demonstrating
nonreactive, low-absorbing, nonmetallic materials contained compliance with the maximum allowable concentration gradi-
within a cabinet or oven capable of maintaining the tempera- ent are acceptable. Normally, a conditioned chamber equili-
brates within several hours after sample loading and start of the
corrosive gas supply. Times longer than 2 h shall be reported in
9
The boldface numbers in parentheses refer to the list of references at the end of the test report; see Section 8. A guide to estimating supply
this standard. requirements is provided in Appendix X1.

2
B 827 – 97 (2003)
This practice involves the use of hazardous materials, proce-
dures, and equipment. The gas concentrations in the test
chamber may be within permissible exposure limits (PEL).11
However, concentrations in the compressed gas cylinders or
permeation devices are often above the PEL, and may exceed
the immediately dangerous to life and health level (IDHL).
This practice does not address safety issues associated with
MFG testing.)
5.1.2.5 Gas Delivery System—The gas delivery system is
comprised of three main parts: gas supply lines, gas control
valves and flow controllers, and a mixing chamber. The gas
delivery system shall be capable of delivering gases at the
required concentrations and rates within the test chamber.
(1) All materials used for the gas transport system must not
interact with the gases to the extent that chamber gas concen-
trations are affected.
(2) Gases, make-up air, and water vapor must be thor-
oughly mixed before gas delivery to the samples under test in
the chambers. Care must be taken to ensure absence of aerosol
formation in the mixing chamber whereby gases are consumed
in the formation of particulates which may interfere with gas
concentration control and may introduce corrosion processes
which are not representative of gaseous corrosion mechanisms.
Aerosol formation may be detected by the presence of a visible
film or deposit on the interior surface of the gas system where
the gases are mixed.
FIG. 1 Schematic Flow-Through Mixed Flowing Gas (MFG) Test (3) Any fogging of the tubing walls or mixing chamber
System walls can be taken to be an indication of a loss of corrosive
gases from the atmosphere. Final mixing of the specified gases
NOTE 1—Guidance: when inlet to outlet concentrations vary by more should occur inside a separate area of, or as close as possible
than 615 %, it usually indicates an overloaded chamber. to, the test chamber so as to ensure thermal equilibration with
5.1.2.2 Clean, Dry, Filtered Air Source— Gases other than the test chamber.
oxygen and nitrogen that are present in the dry air source shall (4) Flow measurement capability is required at the inlet of
be less than or equal to those defined by OHSA Class D limits the chamber and also at the exhaust of negative pressure
with the following additional constraint. Gases other than chambers to ensure the absence of uncalibrated gas streams.
nitrogen, oxygen, carbon dioxide, noble gases, methane, ni- 5.1.2.6 Corrosive Gas Concentration Monitoring System—
trous oxide, and hydrogen shall be less than 0.005 (ppm) by Standard measurement systems for very low level gas concen-
volume total and shall be High Efficiency Particulate Arrestants trations are listed in Table 1, which provides for gases in
(HEPA) filtered. common use in present mixed flowing gas systems, for testing
5.1.2.3 Humidity Source—The humidity source shall use electrical contact performance.
distilled or deionized water, Specification D 1193, Type 1 or (1) Each instrument must be characterized for interference
better, and shall introduce no extraneous material. The humid- with the gases specified, both individually and mixed.
ity source shall be maintained equivalent to Specification (2) Depending on the exact equipment set used, it may not
D 1193 Type II or better, with the exception that electrical be possible to accurately measure the concentration of some
resistivity shall be maintained equivalent to Specification gases, such as chlorine, in combination with any of the other
D 1193 Type IV. The time averaged value of humidity shall be gases.
within 61 % relative humidity of the specified value with (3) The analytic instruments shall be maintained and
absolute variations no greater than 63 % relative humidity calibrated electronically in accordance with the manufacturers’
from the specified value. recommendations. Standard gas sources shall also be calibrated
5.1.2.4 Corrosive Gas Sources—Corrosive (test) gases, in accordance with the manufacturers’ specifications, or in
such as nitrogen dioxide, hydrogen sulfide, chlorine, sulfur accordance with Practice D 3609. Gas concentration analyzers
dioxide, etc. shall be of chemically pure10 grade or better. Such shall be calibrated to standard gas sources in accordance with
gases are frequently supplied in a carrier gas such as nitrogen the manufacturers’ recommendations. They shall be calibrated
which shall be of Pre-Purified 10 grade or better. (Warning—

10 11
Chemically Pure and Pre-Purified are designations of Matheson Gas Co., East Pocket Guide to Chemical Hazards, National Institute for Occupational Safety
Rutherford, NJ, for specific grades of purity of gas. Other vendors such as AIRCO and Health, U.S. Department of Health and Human Service, Publication #85-114,
have equivalent gas purities available sold under different terminology. fifth printing.

3
B 827 – 97 (2003)

FIG. 2 Schematic Vertical Recirculating Mixed Flowing Gas (MFG) Test System

FIG. 3 Schematic Horizontal Recirculating Mixed Flowing Gas (MFG) Test System

before and after each test and whenever the indicated concen- required periodically because the corrosive effects of mixed
tration changes exceed the allowed variation in the test gas environments can affect instrument sensitivity and accu-
specification. racy. The chamber monitoring system must address four test
(4) Control of the temperature and humidity within the test parameters: temperature, humidity, gas concentrations, and
chamber itself is part of the chamber monitoring system which corrosivity.
is described in 5.1.3 5.1.3.1 Temperature Monitoring—Temperature monitoring
NOTE 2—If the chlorine monitor is not being used during the test, it is usually a simple thermocouple or other temperature mea-
need not be calibrated during the test. surement device capable of the required resolution of 0.2°C
5.1.3 Chamber Monitoring System—Chamber monitoring and accuracy of 60.5°C within the temperature range required
systems are required to ensure test reproducibility from one test by the test specification. For test temperatures above 40°C, see
run to the next. Calibration of monitoring instruments is 7.6.5.

4
B 827 – 97 (2003)
TABLE 1 Instrumental Methods for Gaseous Components 6.1.1 Purity of Water—Water for humidity generation shall
NOTE 1—Commercial equipment such as Monitor Labs 8770, Hydro- be equivalent to Type 1 or better of Specification D 1193.
gen Sulfide Converter, in conjunction with Monitor Labs 8850, Sulfur 6.1.2 Carrier Gas—Carrier gas such as nitrogen shall not
Dioxide Analyzer is suitable for this purpose. introduce reactive constituents into the test atmosphere to an
NOTE 2— Commercial equipment such as Monitor Labs 8850, Sulfur amount of more than 5 % of any specified corrosive test
Dioxide Analyzer is suitable for this purpose. atmosphere constituent.
NOTE 3—Commercial equipment such as Monitor Labs 8840, Nitrogen
6.1.3 Clean Filtered Air—Clean filtered air as required for
Oxides Analyzer is suitable for this purpose.
makeup to support the necessary exchange rate, in accordance
Gas Suitable Instrumental Method Suitable Procedure
with 7.6.7.1 (2) is specified in 5.1.2.2.
H2S Photometric or luminescence See Note 1 6.1.4 Corrosive Gases—Corrosive gases shall be chemi-
SO2 Photometric or luminescence Test Methods D 2914, G 91,
D 3449, see Note 2 cally pure9 grade or equivalent.
NO2 Chemiluminescence Method D 3824, see Note 3 6.1.5 Corrosivity Monitor Materials (CMM)—CMM are
Cl2 Electrochemical or Reflectometric Test Method D 2912
comprised of the coupons that are exposed to the test atmo-
The instrument manufacturer’s instructions for delivering samples to the instru-
ments should be followed. sphere for mass gain or coulometric reduction in accordance
with Test Methods B 810 and B 825, respectively, the coated
quartz crystals used for microbalance measurements in accor-
5.1.3.2 Humidity Monitoring—Humidity must be deter- dance with Test Method B 808, resistance monitor materials in
mined by an apparatus with a resolution of 0.5 % relative accordance with Test Method B 826, or other coupons for
humidity and an accuracy of 61 % relative humidity. Test analytical techniques described in Appendix X2.3.
Method D 4230 describes a dew point method which meets this
requirement. For test temperatures above 40°C, see 7.6.5. 7. Procedure
5.1.3.3 Corrosive Gas Monitoring—Chamber corrosive gas 7.1 The following procedure is comprised of requirements
concentration monitoring must be accomplished by provision and other comments provided as a general guide to achieving
of sampling lines from the test chamber to the gas concentra- reproducible results with MFG testing. This procedure is
tion analyzers. These sampling lines must be maintained above compatible with most test facilities; however, differences in
the chamber dew point temperature. The interior of the gas apparatus, test conditions, or local safety requirements may
concentration analyzers shall also be maintained above the necessitate alternative procedures. Any deviations shall be
chamber dew point temperature. For test temperatures above reported with all test results (see Section 8).
40°C, see 7.6.5. 7.2 The procedure is comprised of the following major
5.1.3.4 Chamber Corrosivity Monitoring— Chamber corro- activities: test chamber calibration, sample preparation, test
sivity monitoring can be accomplished by a number of comple- chamber set-up, test chamber start-up, test chamber operation
mentary techniques, none of which provide both a comprehen- during test duration, test chamber shut-down, and reporting
sive analysis of the corrosion process and an instantaneous requirements.
indication of the corrosion rate. Five acceptable techniques are 7.3 Test Chamber Calibration—The spatial uniformity of
as follows: metal coupon corrosion mass gain, corrosion film the corrosivity of test chambers larger than 0.5 m on a side
analysis by coulometric reduction, corrosion film analysis by shall be measured in accordance with Test Method B 810,
electron or X-ray beam analysis, quartz crystal microbalance which describes the required placement scheme for calibration
mass gain, and electrical resistance measurement of corroding samples which are used to determine corrosion rate uniformity
metal conductors (see Note 3). The first three provide infor- over the entire chamber volume. For chambers smaller than 0.5
mation subsequent to the test whereas the last two can be used m on a side or chambers of unusual geometry, use sufficient
in situ in the test chamber to provide information during the samples for corrosivity characterization so as to clearly delin-
test itself. See Appendix X2 for a discussion of these methods. eate the usable chamber working volume as defined in this
It is recommended that the test requester specify chamber paragraph. This profiling shall be done when the chamber is
corrosivity monitoring methods to be used. initially built and after any structural change to the chamber
NOTE 3—A potential sixth method utilizing porous gold coupons is that may affect the flow of test gas over the test samples.Test
under investigation. Method B 810 describes a procedure using mass gain. Alter-
native means to characterize corrosion rates such as Test
5.1.4 Chamber Operating System—The chamber operating
Method B 825, Coulometric Reduction, or Test Method B 808,
system is comprised of equipment and software necessary to
Quartz Crystal Microbalance, in accordance with 5.1.3.4 are
adequately control all of the variables of the test. This will
also acceptable. A minimum of three corrosivity monitors of a
include data logging and alert procedures for operation outside
given type must be used, if possible, in each chamber location.
of desired bounds. Some form of computer control is highly
The average corrosivity for that location must be within 15 %
recommended to assure satisfactory operation during unat-
of the average for the entire chamber. When a single monitor
tended periods and for data tracking for failure analysis in case
has to be used at a location, due to chamber size limitations or
the test is disrupted.
monitor geometry, the average corrosivity for that location
6. Reagents and Materials must be based upon three consecutive calibration runs. These
requirements define the usable chamber working space.
6.1 Materials required to conduct flowing mixed gas tests
are as follows: NOTE 4—Profiling does not remove the necessity to provide and

5
B 827 – 97 (2003)
evaluate CMM for each test run of the test chamber. or in excess of 200 chamber gas exchanges for high-sulfur
7.4 Sample Preparation—Two types of samples are used for tests) to reach 10 % or 0.001 ppm corrosive gas concentration
these tests, CMM and the test samples being evaluated. Prepare levels after chamber shutdown.
CMM in accordance with their respective standards, such as 7.6.4 Chamber Loading:
Test Method B 810. 7.6.4.1 Place the test samples and control materials into the
7.4.1 Prepare the test samples in accordance with any chamber when the samples, materials, and chamber are at
agreement between vendor and user of the samples being ambient temperature and relative humidity in order to avoid
tested. Such preparation shall be consistent with normal visible condensation. Alternatively, samples at chamber tem-
preparations expected when test samples would be exposed to perature can be placed directly into a heated chamber at or
normal application environments in their intended applications below specified humidity.
except when evaluation of preparation methods is the object of 7.6.4.2 For tests which require in situ measurements on the
the test. test samples, install necessary electrical access cabling at this
7.5 Test Chamber Set-Up—Place test samples and CMM in time and make initial measurements, as required by the test
the chamber in a manner that is representative of the way the specification.
test samples would be used in the application environment, if 7.6.5 Chamber Heating—The practical upper limit to the
known. This should be done in a consistent manner, such that test temperature for this procedure is determined by the internal
the test results will be reproducible over time. temperature of the analyzers, including any auxiliary heating,
7.5.1 In general, the samples shall be suspended or held such that condensation of the sampled gas stream will not
with their long dimension parallel to the flow of air and a occur within the instrument. In order to avoid condensation in
minimum of 5 cm away from any surface to avoid boundary the analytical instruments and sampling lines, the relative
layer effects. It is particularly important that no test samples or humidity of the sampled gas mixture in the sampling lines and
CMM be shielded from the source of the pollutant gases by any analytical instruments shall not exceed 80 % relative humidity.
control coupon, test fixture, test samples, test rack, or other This is generally accomplished by heating the sampling lines
obstruction placed upstream. and instruments as required. Manufacturers of the analyzers
7.5.2 In general, when larger systems under test are being should be consulted to determine maximum temperatures at
expressed to a MFG environment, the interior of the system which the analyzers can be maintained. Modifications of this
under test will be underexposed due to the gettering or reaction procedure such as limiting chamber humidity to a wet-bulb
of pollutant gases by the surrounding system surfaces. Under temperature less than the instrument internal temperature
these circumstances, the system should be placed in the during corrosive gas supply settings and subsequent elevation
exposure chamber in a configuration that is consistent with of humidity to specified values may be required for high
exposure in actual field configuration. CMMs should be placed temperature (for example, 70°C), high-humidity corrosive gas
around the system under test. tests.
7.6 Test Chamber Start-Up: 7.6.5.1 Heat the chamber to the specified test temperature, if
7.6.1 Test Conditions—Test conditions such as those given required. A holding time of at least 1 h is recommended to
in Section 8 shall be specified by the test requester. Test ensure temperature equilibration of the test samples. A longer
Method B 845 is a guide to selection of such conditions for time may be necessary for massive assemblies.
specification purposes. 7.6.6 Chamber Humidification:
7.6.2 Avoidance of Condensation—Establish an apparatus 7.6.6.1 Increase the chamber humidity to the specified test
specific start-up and shut-down procedure to avoid visible relative humidity, if required.
water condensation on the test samples and CMM at time of
insertion into the chamber. Such condensation on the parts 7.6.7 Gas Level Setting:
invalidates the test. To avoid condensation at start-up the parts 7.6.7.1 Confirm that temperature and humidity are at equi-
under test shall be at a temperature that is greater than the dew librium at specified test conditions.
point temperature of the chamber at insertion time. To avoid 7.6.7.2 When conducting multiple gas tests with chlorine as
condensation at shut-down the laboratory temperature shall be one of the corrosive gases, chlorine must be the first gas whose
greater than the dew point temperature of the exposure supply setting is established. This is because of interferences
chamber at sample removal time. from other gases which are due to present limitations of the
7.6.3 Chamber Preparation—When contaminants such as chlorine gas monitoring equipment in common use. Allow the
condensed gases (for example, free sulfur or organic material chlorine levels to come to equilibrium in the chamber for at
from test samples) or corrosion particulate deposits are present least 1–2 h.
or suspected, clean the inside of the chamber to reduce the 7.6.7.3 Introduce all the other corrosive gases to the level
concentration of adsorbed gases by wiping the interior walls specified and measure the gas concentrations (see 5.1.2.6), in
with a clean, lint-free cloth before installing samples at the start the test chamber in accordance with 5.1.3.3; adjust the gas
of any test. Residual contamination can affect the accuracy of supply rates and volume exchange rate until the downstream
subsequent chlorine measurements. gas concentrations are within 615 % or 0.003 ppm, whichever
7.6.3.1 An indication of the need for a wipe down would be is larger, of the upstream concentrations and at the gas
an abnormally long time (in excess of 20 chamber gas concentrations specified. Allow to stabilize and repeat mea-
exchanges for low-sulfur (for example, <0.020 ppm H2S) tests surement after 1 to 2 h to confirm gas supply and volume

6
B 827 – 97 (2003)
exchange rate setting. Circulating fans shall be running during Corrosivity monitors such as resistance monitors or quartz
this gas supply setting in recirculating-type chambers. crystal microbalances are recommended to provide an inte-
7.6.7.4 The following points concerning gas concentrations grated continuous assessment of chamber status.
should be noted. 7.7.1 Test Tolerances—Maintain the following tolerances
(1) Inability to achieve 15 % (0.003 ppm) gas concentra- on test parameters unless otherwise specified by the test
tion tolerance between upstream and downstream values may requester:
indicate insufficient exchange rate or excessive loading of test 7.7.1.1 Maintain the temperature within 61°C with a pre-
samples. ferred tolerance of 60.5°C.
(2) Once gas levels are set initially, any change in the gas 7.7.1.2 Maintain the humidity at an average value within
supply system requires confirmation of compliance with the 61 % relative humidity with an absolute variation less than
requirements of 7.6.7.1 (2) and (3) and may necessitate 3 % relative humidity.
resetting of the gas controls; any such actions shall be reported 7.7.1.3 Maintain the gas concentrations within 615 % or
in Section 8. 60.003 ppm, whichever is larger.
(3) For assembly level testing, for example, a disk drive 7.7.1.4 If specified, maintain the corrosivity within 15 % of
assembly or large wiring harness, gas levels should be set the specified value.
upstream of the test object at the maximum exchange capacity 7.7.1.5 Maintain the test duration within 62 % or 62 h,
of the system, with the assembly in place. Record the down- whichever is longer.
stream gas concentrations and report them in the test report as 7.7.2 Psychrometric Monitoring—Continuous or periodic
a deviation, see Section 8. When testing at assembly level, the monitoring of temperature and humidity is required. The
requirement that the gas concentration in the exhaust stream be maximum period between measurements shall be 30 min.
within 15 % (or 0.003 ppm, whichever is larger) of the inlet 7.7.2.1 Air velocity need not be monitored during the test
stream may not be applicable, since it is entirely possible that unless significant changes in sample placement occur during
under operating conditions, exhaust streams from the assembly the test. Some means of verifying that the fans are operating
may be depleted of pollutants due to absorption within the properly is required in recirculating-type chambers in order to
assembly itself. It is recommended that the test requester and ensure that air velocity remains within the tolerance band
test operator discuss the expected deviation from the 15 % specified or the range for which chamber calibration was
concentration variation for assembly testing. obtained.
7.6.8 Air Velocity Confirmation—For tests specifying air 7.7.3 On-Line Control—In addition to monitoring, some
velocity, after test samples are placed in the chamber, and gas type of on-line control is recommended. This allows adjust-
levels and exchange rates are set, measure the velocity of the ments to be made in the gas concentrations dynamically, to
corrosive gas air stream impinging on the test samples between increase the probability of a valid test.
5 and 8 cm upstream of the test samples for compliance with 7.7.4 Test Continuity—The test exposure should be run
the air velocity specified and the allowable tolerance of continuously with as few interruptions as possible, unless
620 %. otherwise specified. Interruptions for removal or replacement
7.6.9 Corrosivity Setting—Where corrosivity is required to of test samples or CMM, during which time chamber condi-
be monitored by means of one or more in situ continuous tions may vary outside of limits defined in 7.7.1, shall not be
monitors such as a quartz crystal microbalance (QCM) or considered deviations as long as total duration of all interrup-
resistance monitor (RM), maintain the corrosivity within the tions is less than 5 % of total test time.
bounds specified by the test specification. Deviations from the
expected corrosivity require immediate attention to the con- NOTE 5—These deviations can be minimized by building a small door
within the main chamber access door to facilitate the removal or addition
trolling test parameters such as temperature, humidity, and gas
of CMM.
concentration to rectify the deviation. Report the inability to
attain the specified corrosivity at the specified test sample 7.7.4.1 Test Integrity—The test shall not be disrupted by the
loading with all other parameters in the specified range as a test addition of new samples for a different test during the operation
deviation in Section 8. of the test. New samples introduce fresh absorbing surfaces
7.6.10 Test Duration—Test duration can be specified by two which can significantly alter the gas concentrations at which
different means. The test may be specified to endure a set the original samples were being tested; such a disruption would
period of time, or it may be specified to endure until a required lead to problems reproducing test results and is unacceptable.
total corrosion, as measured by an in situ corrosivity monitor, 7.8 Test Chamber Shut-Down:
is achieved. 7.8.1 Electrical Power-Down—Discontinue electrical
7.7 Test Chamber Operation—Monitor the test chamber for power to any devices under test and to in situ corrosivity
temperature, humidity, and pollutant gas concentrations to monitors.
demonstrate chamber stability with respect to short-term fluc- 7.8.2 Corrosive Gas Shut-Down—Discontinue corrosive
tuations and long-term drifts. Place CMM in the test chamber gas supply, except for chlorine, if used. Allow chlorine level to
adjacent to the test samples. This will provide a measure of equilibrate in the absence of the other gases. Measure chlorine
chamber corrosivity after the test is completed. For a plane level (also, measure residual levels of other gases) to ensure
array of test samples place a minimum of five CMM, one at compliance with 7.6.7.1 (2) and report if it is outside the test
each corner and one at the center of the array of test samples. specification. Then, discontinue chlorine supply.

7
B 827 – 97 (2003)
7.8.2.1 If high levels of H2S of SO2, or both, are used, it 8. Report
may not be possible to accurately measure the Cl2 concentra- 8.1 The report shall contain the following information:
tion because the sulfur species emitted from the test samples 8.1.1 Facility name.
can interfere in a negative manner to reduce the oxidant-caused 8.1.2 Test engineer.
signal in some chlorine monitors (for example, MAST Oxidant 8.1.3 Test requester.
Monitor). If such interference is suspected, it is necessary to 8.1.4 Date.
remove the test samples prior to verifying the chlorine concen- 8.1.5 Test Samples—Description; number of test samples;
tration. Empty the test chamber of test samples and CMM. condition tested; exposure intervals; and data summary.
Reseal the test chamber and restart the chlorine flow at the 8.1.6 Corrosivity Monitor Materials (CMM)—Description
prior setting. After equilibration of chlorine, measure the (each type); number of CMM; description of CMM placement;
chlorine level and record for inclusion in Section 8. Discon- exposure intervals; data from CMM; procedures used for
tinue chlorine flow. preparation and analysis (for example, in accordance with Test
NOTE 6—If the chlorine level is close to or above the accepted time Method B 810); and equilibration time to stabilize gases at
weighted average (TWA), the testor will have to record the chlorine flow 615 % (or 0.003 ppm), inlet to exhaust, if longer than 2 h.
settings and shut off all corrosive gas supply before opening the chamber 8.1.7 Test Conditions: Levels and Relevant Tolerances—
to the laboratory. The current accepted TWA for chlorine is 500 parts per Gas concentrations; temperature and humidity; air velocity,
billion. It is good laboratory practice to minimize any personnel exposure direction; illumination condition; exchange rate; and test du-
to corrosive gases.12
ration.
7.8.3 Humidity Control—Discontinue humidity generation 8.1.8 Chamber dimensions.
while maintaining chamber temperature, if it is necessary to 8.1.9 Usable chamber working space in accordance with
reduce chamber temperature. When the relative humidity has 7.3.
stabilized at a low level, the chamber temperature may be 8.1.10 Deviations from normal conditions.
reduced in convenient increments while ensuring freedom from 8.1.11 Record of all interruptions (reason and duration).
condensation until the chamber can be safely opened and test
samples and CMM removed from the chamber. 9. Keywords
9.1 air velocity; chlorine; corrosion; corrosive gas testing;
corrosivity; corrosivity monitor; coulometry; environmental;
12
humidity; hydrogen sulfide; mixed flowing gas; nitrogen oxide;
1995–1996 Threshold Limit Values (TLVs) for Chemical Substances and
Physical Agents and Biological Exposure Indices (BEIs), American Conference of
pollutant; pore corrosion; quartz crystal microbalance; resis-
Governmental Industrial Hygienists, Technical Affairs Office, 1330 Kemper tance monitor; sulfur; sulfur dioxide; tarnish; temperature;
Meadow Drive, Cincinnati, OH, 45240. testing

APPENDIXES

(Nonmandatory Information)

X1. ESTIMATING REQUIRED CORROSIVE GAS EXCHANGE RATE

X1.1 The required rate of corrosive gas exchange can be accepted downstream of the exposed copper surface in accor-
estimated from the total gas consumption required to obtain the dance with the requirements of this practice. If the chlorine is
expected corrosion rate for the test being performed. In a being supplied at a concentration of 0.01 ppm in carrier gas,
typical MFG test the initial corrosion rate can be as high as 8 then 0.83 m3 of such supply is required/h/cm2 of exposed
nm of copper corrosion film growth/h over the first 8 h of the copper surface. For 100 cm2 of exposed copper, the gas supply
test. The most conservative assumption of one atom of corro- must be 83 m3/h.
sive gas per atom of copper implies that such a film thickness
requires 2 3 1016 chlorine atoms/h/cm2 of exposed copper X1.2 If half of the film is oxide and half is basic copper
surface, if the entire film is comprised of CuCl. Thus the chloride, Cu2(OH)3Cl, as is more likely, then the chlorine
amount of chlorine supplied to the test chamber must be 2 3 consumption rate is reduced by a factor of 4.7 to 17.7 m3/h/100
1017/h/cm2 if no more than 10 % loss of concentration can be cm2 of exposed copper.

8
B 827 – 97 (2003)

X2. CORROSIVITY MONITORING METHODS

X2.1 Mass Gain Coupons—Test Method B 810 describes a technique is based on a frequency measurement of a resonating
technique for use of copper coupons in chamber monitoring quartz crystal which has been coated with a thin film of
which utilizes mass gain due to formation of corrosion prod- reactive metal such as copper. As the copper corrodes, the mass
ucts from interaction of the corrosive gases with the exposed of the crystal plus copper plus corrosion product increases
surface of the copper coupon. It describes coupon cleaning, leading to a smaller resonant frequency. The frequency shift is
handling, placement, and evaluation procedures. directly related to the amount of corrosion and is sensitive to
less than a monolayer of corrosion product. This sensitivity
X2.2 Coulometric Reduction—Test Method B 825 de- provides an immediate measure of corrosion rate which can be
scribes a procedure for determining the relative amounts of related to gas concentrations or other chamber conditions such
different corrosion film constituents in corrosion films formed as temperature or humidity.
on copper and silver coupons by means of coulometric
reduction techniques. The technique also provides a measure of X2.5 Resistance Monitoring—Test Method B 826 de-
the total amount of copper or silver which has reacted to form scribes the use of a resistance monitoring technique to deter-
corrosion products on the surface of the coupons which have mine the corrosivity of gaseous environments. The technique is
been exposed in the test chamber. based on the comparison of the electrical resistance of two legs
X2.3 Surface Analysis—Surface analysis of corrosion films of a bridge circuit which are exposed to the corrosive gases
has been performed by a number of analytical techniques with the resistance of two legs of the circuit which are shielded
including X-ray diffraction, X-ray emission spectroscopy, from the corrosive gases by the presence of an inert overcoat.
X-ray photoelectron spectroscopy (see Practice E 902), Auger The circuit is formed from thin metal films such that corrosion
electron analysis and secondary ion mass spectroscopy. All of of the film removes metal from the conductive path thus
these techniques yield different data which can be correlated to increasing the resistance. Modifications of this technique have
develop a more complete understanding of corrosion behavior. been successfully used to monitor mixed flowing gas chamber
These techniques are more important when metals other than corrosivity on a real time basis. Sensitivity of the resistance
copper or silver are being examined for susceptibility to mixed bridge can be adjusted by using thinner metal films such that
flowing gas testing because of the absence of extensive data modest corrosion films produce more significant resistance
bases on those other metals in the environments considered shifts.
here. NOTE X2.1—A limitation of the mass gain and resistance techniques is
that the same observed rate of change can be accomplished by different
X2.4 Quartz Crystal Microbalance—Test Method B 808 gas concentrations in a multiple gas chamber. Use of multiple metals
describes the use of the quartz crystal microbalance to provide which are sensitive to different gases is required to assure control of gas
a real time monitor of the corrosion rate of a chamber. The ratios.

REFERENCES

(1) Abbott, W. H., “The Development and Performance Characteristics of (4) Caraballeira, M., Drubay, G., and Caraballeira, A., “Some Parameters
Mixed Flowing Gas Test Environments,” Electrical Contacts-1987, Influencing the Reproducibility of Low Concentration Atmosphere
Proceedings of the Thirty Third IEEE Holm Conference on Electrical Tests,” Electrical Contacts-1984, Proceedings of the Twelfth Interna-
Contacts , IEEE, New York, NY, 1987, pp. 67–78. tional Conference on Electrical Contact Phenomena and the Thirtieth
(2) Rice, D. W., et al., “Atmospheric Corrosion of Copper and Silver,” Annual Holm Conference on Electrical Contacts , Illinois Institute of
Journal of Electrochemical Society, 128, 1981, pp. 275–284. Technology, Chicago, IL, 1984, pp. 69–74.
(3) Graedel, T. E., Franey, J. P., and Kammlott, G. W., “Ozone and (5) Lorenzen, J., “Environmental Monitoring Device for X-ray Determi-
Photon-Enhanced Atmospheric Sulfidation of Copper,” Science, Vol nation of Atmospheric Chlorine, Reactive Sulfur and Sulfur Dioxide,
224, May 11, 1984, pp. 599–601. Adv. X-ray Analysis,” Vol 18, 1975, pp. 568–578.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org).

You might also like