IPC-TM-650 EN 2022 试验方法-- - 第213页
Multiple Headspace Extraction—A Pr ocedure for Quantita- tive Analysis of V olatile Compounds in Solid Samples IPC-TM-650 Number Subject Date Revision Page 3 of 3 Volatile Content of Adhesive Coated Dielectric Films 2.3.…
IPC-TM-650
Number
Subject Date
Revision
Page 2 of 3
Volatile
Content
of
Adhesive
Coated
Dielectric
Films
2.3.37
B
5/98
5.1.2
Evaluation
The
volatile
content
of
each
specimen
is
calculated
as
follows:
Volatile
(W|-WS)(WF-WS)
=
x
100
Content
(%)
(W|-Ws)
5.1.3
Report
The
results
should
be
documented
and
con¬
tain
the
following:
1
.
Certification
that
the
test
was
performed
in
accordance
with
this
test
method.
2.
Identification
of
specimens
tested.
3.
Volatile
content
%
for
each
specimen
tested
and
the
aver¬
age.
Procedure
Method
B
5.2
Calibration
5.2.1
Prepare
two
liquid
calibration
mixtures
as
directed
per
vendor
instructions.
The
mixtures
do
not
need
to
have
these
exact
amounts
but
the
amount
of
each
ingredient
should
be
measured
precisely
to
within
0.0002
grams.
The
mixture
should
be
stored
in
a
suitable
container
with
a
resealable
septa
lid.
Calibration
mixtures
should
be
appropriate
for
vola¬
tiles
present
in
product
tested.
5.2.1.
2
Make
sure
the
mixtures
are
each
well
mixed,
then
determine
the
density
of
the
mixtures
by
any
acceptable
method.
5.2.
1.3
From
each
of
the
mixtures
inject
a
minimum
of
four
different
amounts
(0.5
to
3.0
microliters
each)
into
separate,
previously
prepared,
empty,
sealed
vials.
5.2.1.
4
Allow
each
vial
to
equilibriate
in
the
headspace
unit,
then
inject
each
into
the
chromatograph
and
obtain
an
area
for
each
sample.
5.2.
1.5
Plot
the
areas
vs.
the
amount
(in
milligrams)
of
each
ingredient.
The
eight
points
should
all
lie
on
the
same
straight
line.
5.2.1.
6
Determine
the
response
factor
Rf
(milligrams/area
unit)
for
each
ingredient.
If
the
plot
above
is
not
linear
or
does
not
pass
through
the
origin,
then
it
might
be
necessary
to
have
different
Rf
at
different
amounts.
5.2.2
Sample
5.2.2.1
Cut
and
weigh
a
25.4
mm
square
sample
of
mate¬
rial
to
be
tested.
Place
into
sample
vial
and
seal
tightly.
Equili¬
brate
sample
in
the
headspace
unit
and
then
inject
onto
the
chromatography
column.
Allow
the
chromatogram
to
run
for
eight
minutes.
Note
1
:
Appropriate
time
acd
temperature
dependent
on
product
tested.
5.2.2.2
Calculate
the
amount
of
each
calibrated
peak
using
the
following
equation.
Volatile
%
(i)
=
(Area
(i)
*
Rf
(i)
*
100)/(Wt
*
F)
where:
Area
(i)
=
area
generated
for
ith
calibrated
peak
Rf
(i)
=
response
factor
for
ith
peak
Wa
=
weight
of
sample
(not
including
substrate
—
subtract
out
substrate
weight
by
calculating
the
area
x
the
density
of
the
substrate
under
test
(Ws)
and
subtracting
the
value
from
the
total
sample
weight
(Wt).
Wt
-Ws
=
Wa)
F
二
fraction
of
ingredient
in
film
that
reaches
the
chromatography
relative
to
the
same
frac¬
tion
of
pure
liquid.
5.2.3
Determination
of
F
5.2.3.1
Determination
of
F
—
liq
Prepare
a
mixture
of
ingredients
to
be
tested.
Inject
1
to
2
microliters
of
the
mixture
into
a
sealed
vial.
Equilibrate
in
the
head
space
unit,
then
inject
into
the
chromatograph
and
obtain
the
area
for
each
peak
of
interest.
5.2.3.1.1
Immediately
after
the
injection
is
complete,
vent
the
vial
by
means
of
a
small
syringe
needle
and
replace
the
vial
to
allow
it
to
equilibrate
again.
Again
after
equilibration
inject
the
vial
into
the
chromatograph.
5.2.3.
1.2
Vent
the
vial
a
second
time
and
equilibrate
and
inject
again.
There
should
have
been
three
injections,
each
preceded
by
an
equilibration
and
two
ventings,
one
immedi¬
ately
after
the
first
injection
and
the
other
immediately
after
the
second
injection.
5.2.3.
1.3
Calculate
F
—
ret
—
liq
and
F
_
liq
for
each
ingredi¬
ent
as
follows.
F
—
ret
_
liq
=
(square
root
(area3/area2)
+
area2/area1
)/2
F
—
liq
=
1
-
F
_
ret
_
liq
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.