IPC-TM-650 EN 2022 试验方法.pdf - 第188页

1 Scope This test procedure is designed to measure the level of chloride, bromide, and fluoride present in a soldering flux or paste by Ion Chromatography. 2 Applicable Documents IPC J-STD-004 Requirements for Soldering …

6 Notes

6.1

Ions which may be included for evaluation are as

follows:

Anions:

Bromide

Chloride

Fluoride

Nitrate

Nitrite

Phosphate

Sulfate

Cations:

Ammonium

Calcium

Lithium

Magnesium

Potassium

Sodium

Weak Organic Acids:

Acetate

Adipate

Formate

Glutamate

Malate

Methane Sulfonate

Succinate

Phthalate

Other ions of interest may be present.

6.2 Alternate extraction techniques (change in time, tem-

perature, or extraction solution) may be used as agreed

between user and supplier (AABUS).

6.2.1 Examples of alternate extraction times include the

following:

• Ten-minute extraction (IDEMA specification for metal parts)

• Twenty-four hour extraction

• 16 hour extraction per J-STD-004

6.2.2 Examples of alternate extraction temperatures include

the following:

• Ambient temperature (22±3°C[72±5°F])

6.2.3 Examples of alternate extraction solutions include the

following:

• 10/90 v/v 2-propanol/DI water

• Deionized water

6.3 Ion Chromatography may be a destructive test for

samples due the high temperature liquid extraction and lack of

protection for electrostatic sensitive devices (ESD), moisture

sensitive devices (MSD), and non-hermetically sealed devices.

Note: Caution should be taken when testing samples that

are intended to be deliverable production assemblies.

IPC-TM-650

Number

2.3.28

Subject

Ionic Analysis of Circuit Boards, Ion Chromatography Method

Date

11/12

Revision

Page3of3

Scope

This

test procedure is designed to measure the

level of chloride, bromide, and fluoride present in a soldering

flux or paste by Ion Chromatography.

2 Applicable Documents

IPC J-STD-004

Requirements

for Soldering Fluxes

IPC-TM-650

Test

Methods Manual

2.3.34 Solids Content, Flux

Test Specimens

3.1

Liquid

flux, solder paste, paste flux, extracted solder

preform flux, or cored wire. The reflow/extraction process

should be carried out in accordance with J-STD-004 for the

solder preforms.

Apparatus and Material

4.1

Ion

Chromatograph capable of 50 ppb or better detec-

tion. The equipment and chemistry should be set up and stan-

dardized per the manufacturer’s instructions.

4.2

Hot

Water Bath capable of maintaining 80 ± 5 °C [176 ±

9 °F].

4.3

Clean,

heat sealable bags, i.e., KAPAK® 500 series or

equivalent, with less than 250 ppb extractable contaminants.

(Specify cleanliness level or manufacturers’ part number.)

4.4

Cleanroom

vinyl gloves. (<3 ppm of Cl).

4.5

Deionized

water with a resistivity of at least 18.0

megohm centimeter.

4.6

HPLC

or ASC grade chemicals for eluent and regener-

ant preparation.

4.7

NIST

traceable standards for chloride, bromide and fluo-

ride.

4.8

2-Propanol

(IPA), Electronic grade or better.

4.9

Solder

Pot.

4.10

Analytical

Balance capable of measuring 0.001g.

4.11

mm [1.969 in] mandrel.

4.12

Clean

wire cutters.

4.13

Heat

sealer.

4.14

Ion-free

containers.

4.15

Ultrasonic

bath or magnetic stirrer and stir bar.

4.16

Ion-free

syringe filters.

4.17

Test

Tube.

Procedures

5.1 Liquid Flux / Extracted Flux

5.1.1

Prepare

a solution of 10% by volume isopropyl alcohol

and 90% by volume deionized water and dilute the liquid flux

sample to 200X.

5.1.2

Filter

samples through ion-free syringe filters to

remove particulate prior to analysis.

5.2

Solder Paste/Paste Flux

5.2.1

Weigh

to the nearest 0.001 g., approximately one (1)

gram of solder paste and place it into a tared 165 mm

[6.496 in] by 200 mm [7.874 in] Kapak® bag containing 50 ml

of a solution of 10% by volume isopropyl alcohol and 90% by

volume deionized water.

5.2.2 Prepare

a blank by adding 50 ml of the extract solu-

tion to an empty bag.

5.2.3

Label

and heat seal the bags and place them into a

hot water bath maintained at 80 °C [176 °F].

2215

Sanders Road

Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.28.1

Subject

Halide

Content of Soldering Fluxes and Pastes

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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5.2.4

After

16 hours ± one hour, remove the bags from the

water bath and shake vigorously for 10 seconds to mix the

contents.

5.2.5

Allow

the solutions to cool for 30 minutes minimum

before transferring the extract solutions to ion-free plastic con-

tainers.

5.2.6

Filter

samples through ion-free syringe filters to

remove particulate prior to analysis.

5.3

Flux-Cored Solder Wire

5.3.1

Weigh

approximately fifty (50) grams of the wire

sample.

5.3.2 Wrap

the specimen around a 50 mm [1.969 in] diam-

eter mandrel (Note: Touch the cut ends of the sample with a

soldering iron to seal the sample while cleaning). Place the

resultant sample coil into a beaker of boiling deionized water.

5.3.3

After

approximately five (5) minutes, remove the coil

from the boiling water, rinse with isopropyl alcohol, and allow

to air dry.

5.3.4

After

drying, cut the sample into approximately one (1)

centimeter [0.394 in] length pieces and place inside of a test

tube.

5.3.5

Place

the test tube, with diced sample, in a solder

bath. Thirty (30) seconds after the sample is completely

reflowed, remove the test tube and then allow the solder to

solidify.

5.3.6

Upon

solidification of the solder and before solidifica-

tion of the flux, pour approximately 0.2 grams of the flux into

a test tube of known weight.

5.3.7

Weigh

the second test tube containing the flux and

subtract off the test tube weight to determine the weight of

the flux sample.

5.3.8

Add

a known volume of isopropyl alcohol to the

sample test tube and place the test tube into a sonicator or on

a magnetic stirrer with a stir bar in the test tube for approxi-

mately thirty (30) minutes.

5.3.9

Once

the flux sample is dissolved, dilute the sample

solution such that the overall concentration of isopropyl alco-

hol is approximately 10%.

5.4

Test Method

5.4.1

Extract

solutions shall be analyzed using an Ion Chro-

matograph with a three to five level calibration.

5.4.2

Dilute

extract solutions further with a 10% by volume

isopropyl alcohol solution, if necessary, to lower ion concen-

tration levels within the calibration ranges of the chromato-

graph.

5.5

Calculations

5.5.1 Liquid Flux

5.5.1.1

Determine

the weight of each halide ion in the liquid

flux:

Weight of halide ion (g) in liquid flux =

[ppm from IC (µg/mL)] x

[Dilution factor, if necessary] x

[Volume of dilution solution (ml)] x 10

-6

Note: ‘‘ppm

from IC’’ value is actually specimen value minus

blank value.

5.5.1.2

Determine

the weight of flux solids in the liquid flux:

Weight of flux solids (g) in liquid flux =

[Volume of liquid flux sample (ml)] x

[Density of liquid flux sample (g/ml)] x

[% Solids in liquid flux / 100]

5.5.1.3

Calculate

percent of each halide ion in the nonvola-

tile solid portion of the liquid flux:

Percent of halide ion in solid portion of liquid flux =

[Weight of halide ion (g) in liquid flux] x 100

[Weight

of flux solids (g) in liquid flux]

5.5.2

Solder Paste

5.5.2.1

Determine

the weight of each halide ion in the sol-

der paste flux:

Weight of halide ion (g) in solder paste flux =

[ppm from IC (µg/mL)] x

[Dilution factor, if necessary] x

[Volume of extract solution (mL)] x 10

-6

IPC-TM-650

Number

2.3.28.1

Subject

Halide

Content of Soldering Fluxes and Pastes

Date

06/04

Revision

age2of3

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