IPC-TM-650 EN 2022 试验方法--.pdf - 第191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…

100%1 / 824
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.
5.1.9
Shake the bag to mix the contents. Transfer solution
to virgin sample vials for analysis or pull the sample solution
directly from the bag using a clean syringe for manual injec-
tions.
5.1.10
Remove the test board from the bag, using gloved
hands.
5.2 Calibration Procedure
5.2.1
The ions in the calibration procedure are a minimum.
Other ions may be added to the determination if desired.
5.2.2
A part per million (ppm) is 1 milligram of the ionic spe-
cies (solute, e.g., chloride ion) per 1000 grams of solution.
5.2.3
Prepare or purchase a combination stock anion stan-
dard solution: 5 ppm fluoride, 25 ppm acetate, 50 ppm for-
mate, 20 ppm methanesulfonic acid (MSA), 50 ppm chloride,
50 ppm bromide, 20 ppm nitrate, 200 ppm adipate, 100 ppm
succinate, 20 ppm sulfate, and 20 ppm phosphate.
5.2.3.1
This standard stock can be prepared from 1000
ppm stock solutions using the following formula:
Combine 0.125 ml fluoride; 0.5 ml MSA, nitrate, phosphate,
and sulfate; 0.625 ml acetate; 1.25 ml formate, chloride, and
bromide; 2.5 ml succinate; 5 ml adipate; in a 25 ml volumet-
ric flask. Dilute to volume with 10% 2-propanol / 90% deion-
ized water. The stock solution is stable for several weeks if
kept refrigerated. Warm to room temperature before pipetting.
5.2.4
Prepare or purchase a combination stock cation stan-
dard solution: 5 ppm lithium, 50 ppm sodium, 50 ppm ammo-
nium, 50 ppm potassium, 50 ppm magnesium, and 50 ppm
calcium.
5.2.4.1
This standard stock can be prepared from 1000
ppm stock solutions using the following formula:
Combine 0.125 ml of the lithium standard and 1.25 ml of the
sodium, ammonium, potassium, magnesium, and calcium
standards in a 25 ml volumetric flask. Dilute to volume with
10% 2-propanol / 90% deionized water. The stock solution is
stable for several weeks if kept refrigerated. Warm to room
temperature before pipetting.
5.2.5
Prepare volumes of anion calibration standard solution
for a three point calibration.
5.2.5.1
Standard 1: (0.05 ppm fluoride, 0.25 ppm acetate,
0.5 ppm formate, 0.2 ppm methanesulfonic acid (MSA), 0.5
ppm chloride, 0.2 ppm nitrite, 0.5 ppm bromide, 0.2 ppm
nitrate, 2.0 ppm adipate, 1.0 ppm succinate, 0.2 ppm sulfate,
and 0.2 ppm phosphate) Pipet 1 ml of the combination stock
standard solution to a 100 ml volumetric flask. Add 20 micro-
liters of 1000 ppm nitrite purchased stock solution and dilute
to volume with 10% 2-propanol / 90% deionized water. Mix
well. Prepare fresh daily. (Nitrite is not stable over long periods
of time)
5.2.5.2
Standard 2: (0.1 ppm fluoride, 0.5 ppm acetate, 1.0
ppm formate, 0.4 ppm methanesulfonic acid (MSA), 1.0 ppm
chloride, 0.4 ppm nitrite, 1.0 ppm bromide, 0.4 ppm nitrate,
4.0 ppm adipate, 2.0 ppm succinate, 0.4 ppm sulfate, and
0.4 ppm phosphate) Pipet 1 ml of the combination stock stan-
dard solution to a 50 ml volumetric flask. Add 40 microliters of
1000 ppm nitrite purchased stock solution and dilute to vol-
ume with 10% 2-propanol / 90% deionized water. Mix well.
Prepare fresh daily. (Nitrite is not stable over long periods of
time).
5.2.5.3
Standard 3: (0.2 ppm fluoride, 1.0 ppm acetate, 2.0
ppm formate, 0.8 ppm methanesulfonic acid (MSA), 2.0 ppm
chloride, 0.8 ppm nitrite, 2.0 ppm bromide, 0.8 ppm nitrate,
8.0 ppm adipate, 4.0 ppm succinate, 0.8 ppm sulfate, and
0.8 ppm phosphate) Pipet 1 ml of the combination stock stan-
dard solution to a 25 ml volumetric flask. Add 80 microliters of
1000 ppm nitrite purchased stock solution and dilute to vol-
ume with 10% 2-propanol / 90% deionized water. Mix well.
Prepare fresh daily. (Nitrite is not stable over long periods of
time).
5.2.6
Prepare volumes of cation calibration standard solu-
tion for a three point calibration.
5.2.6.1
Standard 1: (0.05 ppm lithium, 0.5 ppm sodium,
ammonium, potassium, magnesium, and calcium) Pipet 1 ml
of the combination stock cation standard solution to a 100 ml
volumetric flask and dilute to volume with 10% 2-propanol /
90% deionized water and mix well. Prepare fresh daily.
5.2.6.2
Standard 2: (0.1 ppm lithium, 1.0 ppm sodium,
ammonium, potassium, magnesium, and calcium) Pipet 1 ml
of the combination stock standard solution to a 50 ml volu-
metric flask and dilute to volume with 10% 2-propanol / 90%
deionized water and mix well. Prepare fresh daily.
Number
2.3.28.2
Subject
Bare Printed Board Cleanliness by Ion Chromatography
Date
12/2009
Revision
IPC-TM-650
Page
2
of
3