IPC-TM-650 EN 2022 试验方法.pdf - 第214页
1.0 Scope This test method establishes a procedure for determining the thermal decomposition temperature of organic films using thermogravimetric analysis (TGA). 2.0 Applicable Documents ASTM D 618 Standard Practice for …
5.2.3.2
Determination of F__film
Prepare
a film sample in
a vial as standard. Make three injections with venting between
injections and equilibration before each one, just as in the
case of the liquid. The F__ret__film and F__film are calculated
in exactly the same way as F__ret__liq and F__film, except
that the areas used are generated by the film sample.
5.2.3.3
F__liq
and F__film are determined at least eight
times, preferably over a period of several days. Approximately
the same number of liquids as films are tested each day. The
values of F__liq and F__film are averaged separately.
5.2.3.5
Once
determined, F should not change unless the
ingredients change or unless the equilibrium conditions
change.
5.2.3.6
Different
materials will have different values of F.
6 Notes
Multiple
Headspace Extraction—A Procedure for Quantita-
tive Analysis of Volatile Compounds in Solid Samples
,
Kolb,
Auer, and Pospisil, ANGEWANTE CHROMATOGRAPHIE—
APPLIED CHROMATOGRAPHY, January, 1981.
IPC-TM-650
Number
2.3.37
Subject
Volatile
Content of Adhesive Coated Dielectric Films
Date
5/98
Revision
B
P
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1.0
Scope
This
test method establishes a procedure for
determining the thermal decomposition temperature of
organic films using thermogravimetric analysis (TGA).
2.0
Applicable Documents
ASTM D 618
Standard
Practice for Conditioning Plastics and
Electrical Insulating Materials for Testing
ASTM
D 3850
Standard
Test Method for Rapid Thermal
Degradation of Solid Electrical Insulating Materials by Thermo-
gravimetric Analysis
3.0
Test Specimen
The
free films are cut to fit into the
TGA sample pan giving an initial weight of nominally 2-20 mg.
4.0
Apparatus or Material
Thermal
gravimetric analysis
equipment equipped with air, nitrogen purge, capable of
maintaining 5°C heating rate from ambient to 800°C, such as
TA Instruments or Perkin Elmer TGA instruments.
5.0
Procedure
5.1
The
test specimens should be conditioned at 23 ± 2°C
and 50 ± 5% relative humidity for not less than 24 hours prior
to testing. Refer to ASTM D 618 and ASTM D 3850.
5.2
Follow
the manufacturer’s recommendations for equip-
ment startup and calibration.
5.3
Set
the dry nitrogen purge rate at 55 cc/min.
5.4
Allow
the instrument to purge for 30 min.
5.5
Heat
at a rate of 5°C/min from ambient to 150°C.
5.6
Hold
the temperature for 15 min to remove any moisture
from the specimen.
5.7
Heat
at a rate of 5°C/min to 800°C.
5.8
Record
the temperature at which 5% additional weight
loss occurs based on the weight after the 150°C hold.
5.9 Repeat
steps 5.3-5.6 with dry air instead of nitrogen
using a new sample.
5.10
Report
the thermal decomposition temperature, T
max
,
in
degrees Celsius (°C), followed by the evaluation criteria
(e.g., 5% wt. loss), and the atmosphere under which the test
was conducted (e.g., nitrogen), e.g. 185°C (5% wt. loss, nitro-
gen).
6.0
Notes
6.1
Calibration
of the instrument must be carried out
according to the manufacturer’s recommendations. The rate
of flow of the gas in the cell will have a significant effect on the
calibration, therefore the instrument must be calibrated with
the same flow rate used during the test. After the instrument
has been calibrated, the flow rate should not be changed.
6.2
The
surface area of the test specimen will affect the
results. If two specimens of the same material are tested, one
with a large surface area and one with a small surface area,
both of the same mass, the specimen with the smaller surface
area will normally lose weight at a slower rate.
6.3
The
specimen may initially gain weight due to buoyancy
effects.
The
Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road • Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.3.40
Subject
Thermal
Stability
Date
7/95
Revision
Originating Task Group
Deposited Dielectric Task Group (C-13a)
Material
in this Test Methods Manual was voluntarily established by Technical Committees of the IPC. This material is advisory only
and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this
material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.
Equipment referenced is for the convenience of the user and does not imply endorsement by the IPC.
P
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1 Scope The purpose of this test method is to measure the
amount of chlorine and bromine compounds in base materi-
als. This test method is applicable to reinforced base materi-
als with a minimum thickness of 0.3 mm [0.012 in] and to
un-reinforced base materials with a minimum thickness of
0.08 mm [0.0031 in].
A combustion flask is used to extract ionic and covalent halo-
gen from the sample, and Ion Exchange Chromatography is
used for the quantitative analysis of halogen content.
2 Applicable Documents All terms and definitions in this
document conform to IPC-T-50,
Terms and Definitions for
Interconnecting and Packaging Electronic Circuitry.
The IPC Test Method is generated and written, verbatim, from
the IEC 61189-2 TEST 2C12: Total Halogen Content in
Base Materials.
3 Test Specimens Rigid or flexible base materials shall be
used for the test provided they meet the minimum thickness
requirements described in the scope. The copper foil (if appli-
cable) shall be removed from the test specimens by etching
by any industry acceptable etching method or by mechanical
peeling before test.
For reinforced base materials, the number of test specimens
shall not be less than five (5) with a minimum size of 1 cm x
1 cm [0.39 in x 0.39 in]. For unreinforced base materials, the
number of test specimens shall not be less than five (5) with a
minimum size of 1 cmx1cm[0.39 in x 0.39 in].
Wash the specimens thoroughly in distilled or deionized water.
For reinforced base materials, dry the sample at 105 °C [221
°F] +5/- 0 °C [+9 °F/-0 °F] for one hour + 0.25 hour /-0 hour.
For unreinforced base materials, wipe off the water with a lint-
free cloth or paper wiper and leave them to dry at room tem-
perature and atmospheric pressure for a minimum of one
hour.
4 Apparatus & Materials
a. Ion exchange chromatograph with a detection limit of 10
ppm or better.
b. Analytical balance with an accuracy of approximately 1
mg in weight or better.
c. Knife.
d. Tweezers.
e. Vinyl gloves.
f. Lint-free cloth, paper wipers or equivalent.
g. Quantitative filter paper.
h. Combustion flask, or equivalent.
i. Oxygen (99.9 % purity or better).
j. Gas pressure regulator.
k. Flint striker, or another ignition device.
l. Wash bottle.
m. Beaker.
n. Micro-pipette.
o. Flasks (various sizes).
p. Potentiometric titrator for silver nitrate, if necessary.
q. Platinum basket for holding sample.
r. Alkali solution.
s. Ethyl alcohol.
t. Chlorine ion standard solution for chromatograph.
u. Bromine ion standard solution for chromatograph.
v. Silver nitrate titrant, if potentiometric titration using silver
nitrate is used.
5 Procedure
5.1 Combustion Procedure
Weigh the specimen using
the analytical balance and record the result.
Place approximately 50 ml alkali solution in a combustion flask
to act as an absorbent of combustion gas.
Fill the combustion flask with oxygen.
Insert a test specimen into the combustion flask as shown in
Figure 1.
Insert a piece of filter paper into the combustion flask as
shown in Figure 1 to act as a fuse/flame starter.
Apply several drops of ethyl alcohol on the test specimen for
improving the ignition of the specimen and then ignite the
specimen.
3000 Lakeside Drive, Suite 309S
Bannockburn, IL 60015-1219
IPC-TM-650
TEST METHODS MANUAL
Number
2.3.41
Subject
Test Method for Total Halogen Content in Base
Materials
Date
04/06
Revision
Originating Task Group
Halogen Free Materials Subcommittee (4-33)
Material in this Test Methods Manual was voluntarily established by Technical Committees of IPC. This material is advisory only
and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this
material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.
Equipment referenced is for the convenience of the user and does not imply endorsement by IPC.
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