IPC-TM-650 EN 2022 试验方法.pdf - 第202页

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) portio…

1.0

Scope

This

test method provides a measurement of

the flux percentage on flux-coated and/or in flux-cored solder.

2.0

J-STD-006

Requirements

and Test Methods for Electronic

Grade Solder Alloys and Fluxed and Non-fluxed Solid Solders

for Electronic Soldering Applications

3.0

Test Specimen

Use

approximately 200 grams of flux-

coated and/or flux-cored solder. For fluxes whose flux per-

centage is expected to be 1% or more, the test specimen

may be approximately 100 grams. For fluxes whose flux per-

centage is expected to be 2% or more, the test specimen

may be approximately 50 grams.

4.0

Apparatus

4.1

One

hot plate capable of being set to 50+5/-0°C above

the liquidus temperature of the solder sample alloy.

4.2

One

suitably sized pyrex or equivalent beaker.

5.0

Test Procedure

5.1 Preparation for Test

5.1.1

Determine

the liquidus temperature of the solder

specimen alloy from J-STD-006.

5.1.2

Weight

solder sample to the nearest 0.01 gram (W1).

5.1.3

Carefully

pack the solder sample as tightly as possible

in the bottom of the beaker. Weigh the beaker and solder

sample to the nearest 0.01 gram (W2).

5.2

Test

5.2.1

Preheat the hot plate to 50+5/-0°C above the liquidus

temperature of the solder specimen alloy.

5.2.2

Place

the beaker with the solder sample on the hot

plate. Remove the beaker as soon as all of the solder melts

and allow it to cool at room temperature for about 30 minutes.

5.2.3

Using

reagent grade 2-propanol, or other suitable sol-

vent recommended by the solder manufacturer, slight agita-

tion, and gentle heat, thoroughly extract the flux residues from

the beaker. Decant the extraction solution through coarse fil-

ter paper taking care that no solder escapes the beaker.

Repeat the extraction procedure as necessary to remove all

traces of flux residue. Evaporate the remaining solvent from

the beaker by warming under a gentle stream of air until the

residue in the beaker is completely dry.

5.2.4

Weigh

the beaker and melted solder metal to the

nearest 0.01 gram (W3).

5.2.5

Repeat

the flux residue extraction procedure until a

constant final weight W3 is obtained.

5.3

Evaluation

Calculate

the flux percentage using the fol-

lowing formula.

%F=100x(W3-W2)/W1

6.0

Safety

Observe

all approximate safety precautions.

Consult MSDS sheets for safety precautions for chemicals

involved in this test method.

The

Institute for Interconnecting and Packaging Electronic Circuits

2215 Sanders Road • Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.34.1

Subject

Percentage

of Flux on/in Flux-coated and/or

Flux-Cored Solder

Date

1/95

Revision

Originating Task Group

Solder Alloy Task Group (5-24c)

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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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.

Applicable Documents

IPC-TM-650

Test

Methods Manual

2.3.34 Solids Content, Flux

Test Specimen

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.

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

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

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

megohm or better Deionized water.

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

Sanders Road

Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.35

Subject

Halide

Content, Quantitative (Chloride & Bromide)

Date

06/04

Revision

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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TION CONNECTING

ELECTRONICS INDUSTRIES

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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

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

5.3.2

Calculate

halides milliequivalent per gram of flux solids

(nonvolatiles) using the following formula:

Halides, meq/g solids =

VxMx100

Where:

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.

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

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