IPC-TM-650 EN 2022 试验方法--.pdf - 第189页
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-…
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Page 1 of 3
IPC-TM-650
TEST
METHODS
MANUAL
1
Scope
The
purpose
of
the
two
test
methods
is
to
provide
means
for
determining
the
volatile
content
of
adhesive
coated
dielectric
films
used
in
the
manufacture
of
flexible
printed
wir¬
ing.
Method
A
is
a
weight
loss
procedure.
Method
B
is
a
headspace
gas
chromatography
procedure.
2
Applicable
Documents
None
3
Test
Specimen
3.1
Method
A
The
test
specimens
shall
be
squares
of
adhesive
coated
dielectric
film.
The
specimens
shall
be
1
0
cm
x
10
cm.
This
method
is
to
be
used
for
non-aqueous
solvent
systems
only.
3.2
Method
B
Three
specimens
shall
be
prepared:
One
specimen
shall
be
cut
from
the
center
of
the
material
and
one
each
from
each
edge
of
the
material.
Specimens
shall
be
cut
no
closer
than
25.4
mm
from
the
edge
of
the
material.
4
Equipment/Apparatus
4.1
Method
A
4.1.1
Analytical
Balance
Analytical
balance
capable
of
weighing
to
the
nearest
milligram
(0.001
gram).
4.1.2
Test
Chamber
Circulating
air
oven
maintained
at
150℃
±
2.8℃.
4.2
Method
B1
4.2.1
Analytical
Balance
Analytical
balance
capable
of
weighing
to
the
nearest
0.1
milligram
(0.0001
gram).
4.2.2
Sample
Vials
It
is
essential
that
the
septa
are
placed
with
the
Teflon®
side
toward
the
sample
and
that
the
vials
are
sealed
tightly
enough
that
it
is
not
possible
to
turn
the
lid
by
hand.
Number
2.3.37
Subject
Volatile
Content
of
Adhesive
Coated
Dielectric
Films
Date
Revision
5/98
B
Originating
Task
Group
Flex
Peel
Strength
Test
Methods
Task
Group
(D-13A)
4.2.3
Test
Device
A
gas
chromatograph
fitted
with
a
Head
Space
Sampler
and
a
data
acquisition/manipulation
system
capable
of
recording
and
quantitating
gas
chromatograms.
4.2.4
Chromatography
Conditions
Tenax
column
6.35
mm
O.D.
1
.8
m
long.
Injector
temperature:
Product
dependent
Oven
temperature:
Product
dependent
Isothermal
Flame
Ionization
Detector:
Carrier
gas
is
Nitrogen
at
kg/cm2
Adjust
equipment
conditions
for
specific
product
being
tested.
4.2.5
Headspace
Conditions
Temperature
and
dwell
time
dependent
on
product
tested.
5
Procedure
Method
A
5.1
Preparation
5.1.
1.1
Condition
each
specimen
at
50%
±
5%
relative
humidity
(RH)
and
23℃
士
2
℃
for
a
minimum
of
three
hours.
5.
1.1.2
Weigh
each
specimen
to
the
nearest
milligram
(0.001
gram)
[WJ
5.1.
1.3
Subtract
out
substrate
weight
by
calculating
the
area
x
the
density
of
the
substrate
under
test
(Ws).
5.1.
1.4
Hang
each
specimen
from
a
metal
hook
in
the
cir¬
culating
air
oven
at
150℃
±
2.8℃
for
15
±
1
minutes.
5.1.
1.5
Remove
each
specimen
from
the
chamber
and
place
in
a
stabilization
environment
of
50%
土
5%
RH
and
23℃
±
2
℃
for
a
minimum
of
three
hours.
5.1.
1.6
Reweigh
each
specimen
to
the
nearest
milligram
[WF].
5.1.
1.7
Subtract
out
substrate
weight
by
calculating
the
area
x
the
density
of
the
substrate
under
test
(Ws).
1
.
Method
B
requires
proprietary
information
regarding
the
constituents
of
the
material.
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.