IPC-TM-650 EN 2022 试验方法.pdf - 第203页
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…
1
Scope
This
test method is designed to determine the
halide content of fluxes attributable to chlorides and bromides.
The halide content is reported as the weight percentage of
chloride to the solid (nonvolatile) portion of the flux or as mil-
liequivalent per gram of flux solids. A sample of flux or flux
extract is titrated to an end-point and the percentage chloride
or meq/g of halides is calculated.
2
Applicable Documents
IPC-TM-650
Test
Methods Manual
2.3.34 Solids Content, Flux
3
Test Specimen
A
minimum of 50 ml of liquid flux, diluted
paste flux, or diluted solid flux, or 10-50 ml of flux extract from
solder paste, solder preforms or flux-cored wire. The solids
content of the sample must be known or determined by IPC-
TM-650, Test Method 2.3.34.
4
Apparatus and Reagents
4.1 Apparatus
4.1.1
Magnetic
stirrer
4.1.2
Analytical
balance capable of reading to 0.001 g
4.1.3
Pipettes
4.1.4
Burettes
4.1.5
100
ml beakers, Pyrex
4.1.6
125
ml separatory funnel
4.1.7
125
ml Erlenmeyer flasks
4.1.8
1000
ml volumetric flasks
4.1.9
Water
bath
4.2
Reagents
4.2.1
0.1N
silver nitrate, standardized: dissolve 17.000 g sil-
ver nitrate in deionized water and dilute to 1000 ml in a volu-
metric flask.
4.2.2
1M
sodium hydroxide: 40.0 g of sodium hydroxide
diluted to 1000 ml with deionized water in a volumetric flask.
4.2.3
0.2M
nitric acid: add 12.6 ml concentrated (16M) nitric
acid to deionized water and dilute to 1000 ml in a volumetric
flask.
4.2.4
1M
Potassium chromate: 194 g diluted to 1000 ml
using deionized water in a volumetric flask.
4.2.5
0.03M
phenolphthalein solution. (Reagent Grade).
4.2.6
Chloroform
(Reagent Grade).
4.2.7
18
megohm or better Deionized water.
5
Procedures
5.1 Sample Preparation
5.1.1 For Rosin/Resin Fluxes
5.1.1.1
Use
an analytical balance to accurately weigh about
3-5 g of flux sample in a tared 100 ml beaker.
5.1.1.2
Quantitatively
transfer the flux sample to a 125 ml
separatory funnel using three 10 ml aliquots of chloroform.
5.1.1.3
Add
15 ml of deionized water to the funnel and
shake the funnel for 10 seconds.
5.1.1.4
Allow
the funnel to stand until the layers completely
separate.
2215
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Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.3.35
Subject
Halide
Content, Quantitative (Chloride & Bromide)
Date
06/04
Revision
C
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.
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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
age1of1
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TION CONNECTING
ELECTRONICS INDUSTRIES
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