IPC-TM-650 EN 2022 试验方法--.pdf - 第192页

5.1.9 Shake the bag to m ix the contents. Transfer soluti on to virgin sample vi als for anal ysis or pu ll the sample solution directly from t he bag using a clean syringe for manual injec- tions. 5.1.10 Remove the test…

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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
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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
5.2.6.3
Standard 3: (0.2 ppm lithium, 2.0 ppm sodium,
ammonium, potassium, magnesium, and calcium) Pipet 1 ml
of the combination stock standard solution to a 25 ml volu-
metric flask and dilute to volume with 10% 2-propanol / 90%
deionized water and mix well. Prepare fresh daily.
5.2.7
Run a minimum 3 point calibration per the chromato-
graph manufacturer’s recommended methods for both anions
and cations, verifying correct standard concentrations have
been entered into the method.
5.2.8
Adjust the baselines and update the calibration as
required to obtain a good calibration curve. The correlation
factor (R
2
) for the curves should be a minimum of 0.98, with
higher values desirable. Any point on the calibration curve
should not deviate from the expected value by more than ±
10%.
The organic acids standards will typically not form a lin-
ear calibration and a quadratic curve may be required.
5.3 Analytical Procedure
5.3.1
The analysis of the extract solution should be done as
soon as possible after extraction, but
be no longer than
four days from the extraction date.
5.3.2
Start the chromatograph per the manufacturers rec-
ommended method and allow it to come to a stable baseline.
5.3.3
Analyze sample solutions for anion and cation content,
utilizing best analytical technique and laboratory practices.
5.4 Calculation of Results
5.4.1
Values from the chromatograms are typically reported
in parts per million (ppm).
5.4.2 Surface Area Calculation
Record the surface area
of printed board (length x width x 2), e.g., a rectangular
printed board with no cutouts. Alternatively, the surface area
of the printed board can be determined from CAD software or
other machine vision recognition system. Surface area should
be known to three significant figures.
5.4.3
Results are to be expressed as micrograms (µg) of ion
per square centimeter based on the extraction volume and the
calculated sample surface area.
µg/cm
2
=
(SC − BL) x Vol
Area
where:
SC = ppm from IC (µg/mL)
BL = PPM from the bag blank
Vol = final volume (ml)
Area = surface area (cm
2
)
‘‘ppm’’ value is actually specimen value minus blank
value.
5.4.4
Report all ions quantified.
6 Notes
A repeatable and reproducible ionic cleanliness evaluation
method requires some level of skill in accurately running an ion
chromatography unit. The reader may find IPC-WP-008 to be
of use.
Number
2.3.28.2
Subject
Bare Printed Board Cleanliness by Ion Chromatography
Date
12/2009
Revision
IPC-TM-650
Note:
shall
Note:
Page
3
of
3