IPC-TM-650 EN 2022 试验方法.pdf - 第192页
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…
1 Scope This test procedure is designed to measure the
level of anionic and cationic residues on the surface of
unpopulated (bare) printed boards by ion chromatography.
2 Applicable Documents
IPC-WP-008
Setting Up Ion Chromatography Capability
3 Test Specimen Any printed board
4 Apparatus and Materials
4.1
Ion Chromatograph capable of accurately measuring ion
concentration down to 0.5 parts per million (ppm). The equip-
ment and chemistry should be set up and standardized per
the manufacturer’s instructions. The separation column and
eluent composition should be chosen to provide good sepa-
ration of the ions of interest.
4.2 Hot Water Bath capable of maintaining 80±2°C[176 ±
3.6 °F].
4.3 Clean extraction vessels.
4.4 Clean labware.
4.5 Clean gloves, e.g., cleanroom vinyl gloves. (<3 ppm of
Chloride).
4.6 Deionized water with a starting resistivity of at least 16.0
megohm-centimeter.
4.7 HPLC or ACS grade chemicals for eluent and regener-
ant preparation.
4.8 National standard - traceable calibration standards (e.g.,
NIST traceable).
Note: At the time of publication of this test method, a trace-
able industry adipic acid standard does not exist. Future revi-
sions to this test method will indicate such traceability when
available.
4.9 2-Propanol (IPA), 99.5% ACS grade or better.
4.10 Volumetric Flasks (Typically 25, 50, 100, and 1000 ml)
4.11 Precision Pipetting Equipment (such as Eppendorf)
4.12 Ionics-free extract solution sample containers or auto-
sampler vials if an auto-sampler is used with the instrument.
Clean syringes should be used for manual injections.
5 Test Procedures
5.1 Extraction Procedure
Select a low-ion extraction bag
sized to fit the board with approx. 2.5 cm [1.0 in] excess on
each side to minimize required extract solution, with several
inches at the top to allow for air expansion when the bag is
heated.
5.1.2 Use clean gloves when handling the samples to be
tested. Place each sample in an extraction bag.
5.1.3 Prepare a 10%/90% volume/volume 2-propanol /
deionized water solution for the extraction.
5.1.4 Add a known volume of the extraction solution to
the extraction bag covering the printed board (approx. 0.5
mL/cm
2
of surface area).
5.1.5 Add the same volume of extraction solution to an
empty bag of the same lot for use as a blank.
5.1.6 Suspend the bags into the 80±2°C[176 ± 3.6 °F]
water bath allowing the water to force most of the air from the
bags. Do not allow any of the water from the water bath into
the extract solution in the bags. Fold the top of the bags over
the suspending bar and clip in place with binder clips. This will
minimize solvent loss during the extraction, yet not create a
sealed bag. Alternatively, the bags may be heat sealed after
forcing most of the air from the bag.
5.1.7 Allow the sample to soak for one hour (-0 min., +5
min.).
5.1.8 Remove the bags from the water bath and allow the
bags/solution to cool to room temperature.
3000 Lakeside Drive, Suite 309S
Bannockburn, IL 60015-1249
IPC-TM-650
TEST METHODS MANUAL
Number
2.3.28.2
Subject
Bare Printed Board Cleanliness by Ion
Chromatography
Date
12/2009
Revision
Originating Task Group
Ion Chromatography/Ionic Conductivity Task Group
(5-32a)
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.
Page1of3
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.
IPC-TM-650
Number
2.3.28.2
Subject
Bare Printed Board Cleanliness by Ion Chromatography
Date
12/2009
Revision
Page2of3
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%.
Note: 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 shall 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
)
Note: ‘‘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.
IPC-TM-650
Number
2.3.28.2
Subject
Bare Printed Board Cleanliness by Ion Chromatography
Date
12/2009
Revision
Page3of3