IPC-TM-650 EN 2022 试验方法.pdf - 第204页

1 Scope This test method is designed to determine the presence (if any) of fluoride(s) in soldering flux by visual exami- nation after placement of a drop of liquid test flux in a zirco- nium - alizarin purple lake. 2 Ap…

100%1 / 824
5.1.1.5
Draw
off the bottom (chloroform) layer into a beaker
and save for the next extraction.
5.1.1.6
Transfer the top (water) layer to a 125 ml Erlenmeyer
flask.
5.1.1.7 Transfer the chloroform layer from the beaker to the
funnel and repeat the extraction with 15 ml of water two more
times, each time adding the water extract portion to the flask.
5.1.1.8 Using
a water bath, heat the water extract in the
Erlenmeyer flask to expel any chloroform which may be
present.
5.1.1.9
Do
not heat above 80 °C [176 °F]. Allow solution to
cool to room temperature.
5.1.2
For Organic and Inorganic (Water Soluble) Fluxes
5.1.2.1
Use
an analytical balance to accurately weigh about
3-5 g of flux sample in a tared 125 ml Erlenmeyer flask.
5.1.2.2
Add
50 ml deionized water.
5.2
Test
5.2.1
Add
two drops of 0.03 M phenolphthalein solution to
the Erlenmeyer flask (from step 5.1.1.9 or 5.1.2.2).
5.2.2
Add
1 M sodium hydroxide until the solution turns red.
Add 0.2 M nitric acid dropwise until the red color is just com-
pletely discharged.
5.2.3
Dilute
to about 60 ml with deionized water.
5.2.4
Add
six drops of 1 M potassium chromate and titrate
with standardized 0.1N silver nitrate to the red-brown end
point.
5.3 Calculations
5.3.1
Calculate
the weight percentage of halides as chloride
based on flux solids content, using the following formula:
Halides, as % chlorides =
3.55VNx100
mS
5.3.2
Calculate
halides milliequivalent per gram of flux solids
(nonvolatiles) using the following formula:
Halides, meq/g solids =
VxMx100
mS
Where:
V
is the volume of 0.1N silver nitrate in ml.
N is the normality of silver nitrate solution.
m is the mass (weight) of flux sample in grams.
S is the percentage of solids (nonvolatiles) of the flux.
6
Notes
6.1 Safety
Observe
all appropriate precautions on MSDS
for chemicals involved in this test method.
IPC-TM-650
Number
2.3.35
Subject
Halide
Content, Quantitative (Chloride & Bromide)
Date
06/04
Revision
C
P
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1
Scope
This
test method is designed to determine the
presence (if any) of fluoride(s) in soldering flux by visual exami-
nation after placement of a drop of liquid test flux in a zirco-
nium - alizarin purple lake.
2
Applicable Documents
IPC J-STD-004
Requirements
for Soldering Fluxes
3
Test Specimen
3.1
A
minimum of 10 ml of first article or production speci-
men of liquid flux, solder paste, paste flux, or extracted flux
from preform or wire.
3.2
The
extraction of preforms or wire should be carried out
in accordance with J-STD-004.
3.3
For
paste flux or solder paste, dilute the sample in
2-propanol or another suitable solvent. A minimum amount of
solvent should be used just allowing for the sample to be
dropped from a dropper.
Note: The solvent used in dilution/extraction must be water
miscible.
4
Apparatus and Reagents
4.1 Apparatus
4.1.1
White
spot plate
4.1.2
Glass
droppers
4.1.3
Glass
rods
4.2
Reagents
4.2.1
Zirconium nitrate solution: 0.05 g dissolved in 50 ml of
deionized water.
4.2.2
Sodium
alizarin sulfate solution: 0.05 g dissolved in 50
ml of deionized water acidified with 10 ml of hydrochloric acid.
5
Procedure
5.1 Preparation
Prepare
a fresh zirconium - alizarin purple
lake in three spots of the white spot plate by adding one drop
each of zirconium nitrate and sodium alizarin sulfate solutions.
5.2
Test
5.2.1
Add
one drop of the test flux to each of the spots.
5.2.2
Mix
each spot with a clean glass rod.
5.2.3
Examine
for any color change.
5.3
Evaluation
A
change in color of the lake from purple to
yellow is an indication of the presence of fluoride(s). A color
change is typically seen at concentrations between 100 and
150 parts per million fluoride.
6
Notes
6.1 Safety
Observe
all appropriate precautions on MSDS
for chemicals involved in this test method.
2215
Sanders Road
Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.3.35.1
Subject
Fluorides
By Spot Test, Fluxes-Qualitative
Date
06/04
Revision
A
Originating Task Group
Flux Specifications Task Group (5-24a)
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.
P
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1
Scope
This
test method is used to determine the con-
centration of fluorides in soldering flux. The fluoride content is
reported as the weight percentage of fluoride to the non-
volatile portion of the flux. Ion specific electrodes are used for
the determination. This method uses Orion equipment and
solutions.
2
Applicable Documents
IPC-TM-650
Test
Methods Manual
2.3.34 Solids Content, Flux
IPC-J-STD-004
Requirements
for Soldering Fluxes
3
Test Specimen
3.1
A
minimum of 50 ml of first article or production speci-
men of liquid flux or prepared flux solution.
3.2
For
solid or paste flux, 50 ml of the diluted material.
3.3
For
solder paste, preform, and cored wire, 50 ml of the
extracted flux.
3.4
The
solids content of the sample must be known or
determined by IPC-TM-650, Test Method 2.3.34.
Note: Recommended procedures for dilution of solid or paste
flux, and extraction of solder paste, cored wire, or preforms,
can be found in J-STD-004.
4
Apparatus and Reagents
4.1 Apparatus
4.1.1
Autocalibrating
ion analyzer.
4.1.2
Fluoride
specific electrode.
4.1.3
Double
junction reference electrode.
4.1.4 Magnetic
stirrer and stir bars.
4.1.5
250
ml and 500 ml beakers, glass or polypropylene.
4.1.6 Funnel
stand and funnel.
4.1.7
50
ml graduated cylinders.
4.1.8
100
ml and 1000 ml volumetric flasks.
4.1.9
10
ml and 100 ml pipettes.
4.1.10
Analytical
balance capable of 0.001 g.
4.2
Reagents
4.2.1
Deionized
water with a resistivity of at least 18.0
megohm centimeter.
4.2.2
Sodium
fluoride, reagent grade.
4.2.3 Chloroform,
reagent grade.
4.2.4
Total
ionic strength adjustment buffer.
4.2.5
Whatman
#41 ashless filter paper, or equivalent.
5
Procedure
5.1 Sample Preparation - Water Soluble Flux
Depend-
ing
on the expected concentration of fluoride, use the follow-
ing amount of sample and deionized water.
ppm
Fluoride Sample ml DI Water ml
0.1-1.0
25 50
1.0-10.0 5 50
5.1.1
Tare
a beaker and add sample. Record the weight of
the flux to 0.001 gram.
5.1.2
Add
DI water and mix with stirrer for 10 minutes. Stop
mixing and allow to stand for five minutes.
5.1.3
Pour
solution through filter paper in funnel into a clean
beaker. Allow sample to drain completely.
5.2
Sample Preparation - Nonwater Soluble Flux
5.2.1
Depending
on the expected concentration of fluoride,
use the following amount of sample and chloroform.
2215
Sanders Road
Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.3.35.2
Subject
Fluoride
Concentration, Fluxes-Quantitative
Date
06/04
Revision
A
Originating Task Group
Flux Specifications Task Group (5-24a)
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.
P
age1of3
ASSOCIA
TION CONNECTING
ELECTRONICS INDUSTRIES
®
电子技术应用　　　　　　　ｗｗｗ．ＣｈｉｎａＡＥＴ．ｃｏｍ