IPC-TM-650 EN 2022 试验方法-- - 第214页
ASTM D 618 ASTM D 38 50 The Institute for Int erconnecting and Packaging E lectronic Circuits 2215 S anders Road • Northbrook, IL 60062-6135 Material in this T est M ethods Manual was vol untaril y establis hed by T echn…
Multiple Headspace Extraction—A Procedure for Quantita-
tive Analysis of Volatile Compounds in Solid Samples
IPC-TM-650
Number
Subject Date
Revision
Page 3 of 3
Volatile
Content
of
Adhesive
Coated
Dielectric
Films
2.3.37
B
5/98
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
,
Kolb,
Auer,
and
Pospisil,
ANGEWANTE
CHROMATOGRAPH
IE-
APPLIED
CHROMATOGRAPHY,
January,
1981.
ASTM D 618
ASTM D 3850
The Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road • Northbrook, IL 60062-6135
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.
Page 1 of 1
IPC-TM-650
TEST
METHODS
MANUAL
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
Standard
Practice
for
Conditioning
Plastics
and
Electrical
Insulating
Materials
for
Testing
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
℃
heating
rate
from
ambient
to
800℃,
such
as
TA
Instruments
or
Perkin
Elmer
TGA
instruments.
5
.0
Procedure
5.1
The
test
specimens
should
be
conditioned
at
23
±
2
℃
and
50
土
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.
Number
2.3.40
Subject
Thermal
Stability
Date
7/95
Revision
Originating
Task
Group
Deposited
Dielectric
Task
Group
(C-13a)
5.6
Hold
the
temperature
for
1
5
min
to
remove
any
moisture
from
the
specimen.
5.7
Heat
at
a
rate
of
5
℃/min
to
800℃.
5.8
Record
the
temperature
at
which
5%
additional
weight
loss
occurs
based
on
the
weight
after
the
150℃
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,
Tmax,
in
degrees
Celsius
(
℃),
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℃
(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.
5.5
Heat
at
a
rate
of
5
℃/min
from
ambient
to
150℃.
6.3
The
specimen
may
initially
gain
weight
due
to
buoyancy
effects.
Terms and Definitions for
Interconnecting and Packaging Electronic Circuitry.
IEC 61189-2 TEST 2C12: Total Halogen Content in
Base Materials.
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.
Page 1 of 3
r
ASSOCIATION
CONNECTING
/
ELECTRONICS
INDUSTRIES
®
3000
Lakeside
Drive,
Suite
309S
Bannockburn,
IL
6001
5-1
21
9
IPC-TM-650
TEST
METHODS
MANUAL
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,
The
I
PC
Test
Method
is
generated
and
written,
verbatim,
from
the
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
cm
x
1
cm
[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
[221
°F]
+5/-
0
[+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
1
0
ppm
or
better.
b.
Analytical
balance
with
an
accuracy
of
approximately
1
mg
in
weight
or
better.
Number
2.3.41
Subject
Test
Method
for
Total
Halogen
Content
in
Base
Materials
Date
Revision
04/06
Originating
Task
Group
Halogen
Free
Materials
Subcommittee
(4-33)
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.
I.
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.