IPC-TM-650 EN 2022 试验方法--.pdf - 第193页

5.2 .6.3 Stan dard 3 : (0. 2 pp m li thi um, 2 .0 p pm s odium , ammonium, p otassium, magnesium, and calci um) Pipe t 1 ml of the c omb ination stock standard solution to a 2 5 ml volu- metric flask and dil ute to volum…

100%1 / 824
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
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 1
r
ASSOCIATION
CONNECTING
/
ELECTRONICS
INDUSTRIES
®
221
5
Sanders
Road
Northbrook,
IL
60062-6135
IPC-TM-650
TEST
METHODS
MANUAL
1
Scope
This
test
method
is
used
to
measure
pH
in
anhy¬
drous
fluorocarbon
azeotropes
and
blends
in
cleaning
and
defluxing
equipment.
This
method
does
not
work
in
the
presence
of
organic
acid
acceptors
normally
present
with
chlorinated
solvents,
namely
1,1,1
-trichloroethane
and
trichloroethylene.
2
Applicable
Documents
None
3
Test
Specimen
3.1
Approximately
25
ml
samples
of
solvent
are
taken
from
the
boiling
sump
and
condensate
rinse
sump
of
the
operating
fluorocarbon
vapor
defluxer
or
degreaser
and,
for
comparison
purposes,
from
the
virgin
solvent
supply.
4
Equipment/Apparatus
4.1
pH
indicator
sticks
TM
"colorpHast”®
cat.
#9590
avail¬
able
from
MOB
Manufacturing
Chemists
Inc.,
2909
Highland
Ave.,
Cincinnati,
OH
45212
4.2
Screw
cap
glass
vials
(50
ml,
three
or
six
required
per
test)
4.3
Graduated
glass
cylinders
(50
ml,
three
required
per
test)
Caution:
Plastic
is
sometimes
attacked
by
solvents
such
as
acetone,
methylene
chloride
azeotropes.
5
Procedure
5.1
Transfer
25
ml
of
virgin
solvent
to
a
clean
vial
using
a
clean,
dry
graduated
cylinder,
insert
a
"colorpHast”®
plastic
strip,
and
cap
the
vial.
Number
2.3.30
Subject
Solvent
pH
Determination
in
Anhydrous
Fluorocarbons
Solvents
Date
Revision
11/81
A
Originating
Task
Group
N/A
5.2
Repeat
5.1,
sampling
the
defluxer
or
degreaser
boiling
sump.
5.3
Repeat
5.1
,
sampling
the
condensate
or
rinse
sumps.
5.4
Allow
the
test
vials
to
stand
30
minutes.
5.5
Compare
the
colors
on
the
test
sticks
with
the
“color-
pHast”®
color
key
and
record
the
matching
pH
value.
5.6
Discard
the
"colorpHast”®
indicator
sticks
and
vials
after
emptying
the
solvent
into
the
boiling
sump.
5.7
Rinse
the
graduated
cylinders
with
virgin
solvent,
empty
into
the
boiling
sump,
and
allow
to
dry
for
reuse.
5.8
With
fl
uorocarbon/acetone
and
fluorocarbon/methylene
chloride
azeotropes
or
mixtures,
which
attack
the
indicator
adhesive,
repeat
the
above
steps,
but
with
two
vials
of
each
sample.
Cut
the
bottom
two
color
squares
off
three
"color-
pHast"®
sticks
and
discard
the
remainder
of
the
stick.
Put
one
square
of
each
color
in
samples
from
5.1
,
5.2,
and
5.3
sources
and
complete
steps
5.4
through
5.7.
5.9
Interpretation
of
Results
If
pH
is
above
5.5,
this
is
an
acceptable
condition.
If
pH
is
less
than
5.5,
the
solvent
is
contaminated
by
an
accumulation
of
activated
flux
residues,
organic
acids,
or
thermal
degradation
products
of
the
solvent.
This
requires
inspection
to
establish
the
need
for
cleaning
of
the
equipment
and
for
recovery
of
the
solvent.