IPC-TM-650 EN 2022 试验方法.pdf - 第211页
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 pro…
0SHA
recommended exposure limits for chlorinated sol-
vents (all in parts per million).
Chlorinated
Solvent
Perchloroethylene
Trichloroethylene
1,1,1-Trichloroethane
Methylene
Chloride
OSHA
8Hr
TWA
1
100
100
350
500
ACGIH
TLV
2
50
50
350
100
ACC
3
200
200
450
a
1000
AMP
4
300/5 min. in any 3 hrs.
200/5 min. in any 2 hrs.
2000/5 min. in any 2 hrs.
a. No limits established by OSHA. ACGIH recommends a short term exposure limit (STEL) of
450 ppm.
(1) TWA–Time Weighted Average
(2) ACGIH–American Conference of Governmental Hygienists
TLV–Threshold limit values from ACGIH Handbook, 83/84
(3) ACC–Acceptable Ceiling Concentration
(4) AMP–Acceptable Maximum Peak
6.4
First Aid
6.4.1 Eye Contact
Rinse
eyes with running water for at
least 30 minutes. Prompt medical attention is essential.
6.4.2
Skin Contact
Flush
the area thoroughly with water.
Wash clothing before reusing it.
6.4.3
Oral Ingestion
DO
NOT INDUCE VOMITING. Call a
physician or transport the worker to an emergency facility.
6.4.4
Inhalation
Remove
the worker to fresh air if the
worker starts feeling dizzy or light-headed. Contact a physi-
cian or transport the worker to a medical facility. If breathing
stops, give mouth-to-mouth resuscitation. Administer oxygen
when breathing starts (see 6.3.2 for chlorinated solvent expo-
sure limits).
6.4.5
Additional Help
For
any additional chemical related
medical help, call Chemtree Emergency at 800) 424-9000. In
Canada call (collect) Canutel (613) 996-6666.
6.5
All
equipment and chemicals used were purchased from
Van Waters and Rogers standard lab supply catalog.
6.6
This
test is designed for the base chlorocarbons only;
therefore, discretion should be used when testing bipolar sol-
vents.
6.7
Specific Questions
Any
specific questions can be
referred to Dow Chemical U.S.A., Inorganic Chemicals
Department, Technical Service and Development, Midland,
Mich. 48640.
IPC-TM-650
Number
2.3.36
Subject
Acid
Acceptance of Chlorinated Solvents
Date
10/85
Revision
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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 10 cm
x10cm.
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°C ± 2.8°C.
4.2
Method B
1
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.
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/cm
2
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°C ± 2°C for a minimum of three hours.
5.1.1.2
Weigh each specimen to the nearest milligram
(0.001 gram) [W
1
].
5.1.1.3
Subtract
out substrate weight by calculating the
area x the density of the substrate under test (W
s
).
5.1.1.4
Hang
each specimen from a metal hook in the cir-
culating air oven at 150°C ± 2.8°C for 15 ± 1 minutes.
5.1.1.5
Remove
each specimen from the chamber and
place in a stabilization environment of 50% ± 5% RH and
23°C ± 2°C for a minimum of three hours.
5.1.1.6
Reweigh
each specimen to the nearest milligram
[W
F
].
5.1.1.7
Subtract
out substrate weight by calculating the
area x the density of the substrate under test (W
s
).
1.
Method B requires proprietary information regarding the constituents of the material.
The
Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road • Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.3.37
Subject
Volatile
Content of Adhesive Coated Dielectric
Films
Date
5/98
Revision
B
Originating Task Group
Flex Peel Strength Test Methods Task
Group (D-13A)
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.
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5.1.2
Evaluation
The
volatile content of each specimen is
calculated as follows:
Volatile
Content (%)
=
(W
I
−W
S
)(W
F
−W
S
)
(W
I
−W
S
)
x
100
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 and 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 (W
s
)
and subtracting the value from the
total sample weight (Wt). Wt −Ws = Wa)
F = 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
IPC-TM-650
Number
2.3.37
Subject
Volatile
Content of Adhesive Coated Dielectric Films
Date
5/98
Revision
B
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