IPC-TM-650 EN 2022 试验方法.pdf - 第191页

1 Scope This test procedure is designed to measure the level of anionic and cationic residues on the surface of unpopulated (bare) printed boards by ion chromatography. 2 Applicable Documents IPC-WP-008 Setting Up Ion Ch…

5.5.2.2

Determine

the weight of flux solids in the solder

paste flux:

Weight of flux solids (g) in solder paste flux =

[Weight of solder paste sample (g)] x

[% Flux in solder paste / 100] x

[% Solids in paste flux / 100]

5.5.2.3 Calculate

the percentage of each halide ion in the

nonvolatile solid portion of the liquid flux:

Percent of halide ion in solid portion of solder paste flux =

[Weight of halide ion (g) in solder paste] x 100

[Weight

of flux solids (g) in solder paste]

5.5.3

Flux-Cored Solder Wire

5.5.3.1

Determine

the weight of each halide ion in the sol-

der wire flux:

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

[ppm from IC (µg/mL)] x

[Dilution factor, if necessary] x

[Volume of dilution solution (ml)] x 10

-6

5.5.3.2

Determine

the weight of flux solids in the solder wire

flux:

Weight of flux solids (g) in solder wire flux =

[Weight of flux sample (g)] x [% Solids in flux / 100]

5.5.3.3 Calculate percent of each halide ion in the nonvola-

tile solid portion of the solder wire flux:

Percent of halide ion in solid portion of solder wire flux =

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

[Weight

of flux solids (g) in flux]

Notes

6.1

When

establishing an ion chromatography method, the

containers utilized for extraction and sample processing

should be evaluated to confirm that error is not introduced by

the chosen ‘‘ion-free’’ containers.

6.2

Safety

Observe

all appropriate precautions on MSDS

for chemicals involved in this test method.

IPC-TM-650

Number

2.3.28.1

Subject

Halide

Content of Soldering Fluxes and Pastes

Date

06/04

Revision

age3of3

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1 Scope This test procedure is designed to measure the

level of anionic and cationic residues on the surface of

unpopulated (bare) printed boards by ion chromatography.

2 Applicable Documents

IPC-WP-008

Setting Up Ion Chromatography Capability

3 Test Specimen Any printed board

4 Apparatus and Materials

4.1

Ion Chromatograph capable of accurately measuring ion

concentration down to 0.5 parts per million (ppm). The equip-

ment and chemistry should be set up and standardized per

the manufacturer’s instructions. The separation column and

eluent composition should be chosen to provide good sepa-

ration of the ions of interest.

4.2 Hot Water Bath capable of maintaining 80±2°C[176 ±

3.6 °F].

4.3 Clean extraction vessels.

4.4 Clean labware.

4.5 Clean gloves, e.g., cleanroom vinyl gloves. (<3 ppm of

Chloride).

4.6 Deionized water with a starting resistivity of at least 16.0

megohm-centimeter.

4.7 HPLC or ACS grade chemicals for eluent and regener-

ant preparation.

4.8 National standard - traceable calibration standards (e.g.,

NIST traceable).

Note: At the time of publication of this test method, a trace-

able industry adipic acid standard does not exist. Future revi-

sions to this test method will indicate such traceability when

available.

4.9 2-Propanol (IPA), 99.5% ACS grade or better.

4.10 Volumetric Flasks (Typically 25, 50, 100, and 1000 ml)

4.11 Precision Pipetting Equipment (such as Eppendorf)

4.12 Ionics-free extract solution sample containers or auto-

sampler vials if an auto-sampler is used with the instrument.

Clean syringes should be used for manual injections.

5 Test Procedures

5.1 Extraction Procedure

Select a low-ion extraction bag

sized to fit the board with approx. 2.5 cm [1.0 in] excess on

each side to minimize required extract solution, with several

inches at the top to allow for air expansion when the bag is

heated.

5.1.2 Use clean gloves when handling the samples to be

tested. Place each sample in an extraction bag.

5.1.3 Prepare a 10%/90% volume/volume 2-propanol /

deionized water solution for the extraction.

5.1.4 Add a known volume of the extraction solution to

the extraction bag covering the printed board (approx. 0.5

mL/cm

of surface area).

5.1.5 Add the same volume of extraction solution to an

empty bag of the same lot for use as a blank.

5.1.6 Suspend the bags into the 80±2°C[176 ± 3.6 °F]

water bath allowing the water to force most of the air from the

bags. Do not allow any of the water from the water bath into

the extract solution in the bags. Fold the top of the bags over

the suspending bar and clip in place with binder clips. This will

minimize solvent loss during the extraction, yet not create a

sealed bag. Alternatively, the bags may be heat sealed after

forcing most of the air from the bag.

5.1.7 Allow the sample to soak for one hour (-0 min., +5

min.).

5.1.8 Remove the bags from the water bath and allow the

bags/solution to cool to room temperature.

3000 Lakeside Drive, Suite 309S

Bannockburn, IL 60015-1249

IPC-TM-650

TEST METHODS MANUAL

Number

2.3.28.2

Subject

Bare Printed Board Cleanliness by Ion

Chromatography

Date

12/2009

Revision

Originating Task Group

Ion Chromatography/Ionic Conductivity Task Group

(5-32a)

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.

Page1of3

5.1.9 Shake the bag to mix the contents. Transfer solution

to virgin sample vials for analysis or pull the sample solution

directly from the bag using a clean syringe for manual injec-

tions.

5.1.10 Remove the test board from the bag, using gloved

hands.

5.2 Calibration Procedure

5.2.1

The ions in the calibration procedure are a minimum.

Other ions may be added to the determination if desired.

5.2.2 A part per million (ppm) is 1 milligram of the ionic spe-

cies (solute, e.g., chloride ion) per 1000 grams of solution.

5.2.3 Prepare or purchase a combination stock anion stan-

dard solution: 5 ppm fluoride, 25 ppm acetate, 50 ppm for-

mate, 20 ppm methanesulfonic acid (MSA), 50 ppm chloride,

50 ppm bromide, 20 ppm nitrate, 200 ppm adipate, 100 ppm

succinate, 20 ppm sulfate, and 20 ppm phosphate.

5.2.3.1 This standard stock can be prepared from 1000

ppm stock solutions using the following formula:

Combine 0.125 ml fluoride; 0.5 ml MSA, nitrate, phosphate,

and sulfate; 0.625 ml acetate; 1.25 ml formate, chloride, and

bromide; 2.5 ml succinate; 5 ml adipate; in a 25 ml volumet-

ric flask. Dilute to volume with 10% 2-propanol / 90% deion-

ized water. The stock solution is stable for several weeks if

kept refrigerated. Warm to room temperature before pipetting.

5.2.4 Prepare or purchase a combination stock cation stan-

dard solution: 5 ppm lithium, 50 ppm sodium, 50 ppm ammo-

nium, 50 ppm potassium, 50 ppm magnesium, and 50 ppm

calcium.

5.2.4.1 This standard stock can be prepared from 1000

ppm stock solutions using the following formula:

Combine 0.125 ml of the lithium standard and 1.25 ml of the

sodium, ammonium, potassium, magnesium, and calcium

standards in a 25 ml volumetric flask. Dilute to volume with

10% 2-propanol / 90% deionized water. The stock solution is

stable for several weeks if kept refrigerated. Warm to room

temperature before pipetting.

5.2.5 Prepare volumes of anion calibration standard solution

for a three point calibration.

5.2.5.1 Standard 1: (0.05 ppm fluoride, 0.25 ppm acetate,

0.5 ppm formate, 0.2 ppm methanesulfonic acid (MSA), 0.5

ppm chloride, 0.2 ppm nitrite, 0.5 ppm bromide, 0.2 ppm

nitrate, 2.0 ppm adipate, 1.0 ppm succinate, 0.2 ppm sulfate,

and 0.2 ppm phosphate) Pipet 1 ml of the combination stock

standard solution to a 100 ml volumetric flask. Add 20 micro-

liters of 1000 ppm nitrite purchased stock solution and dilute

to volume with 10% 2-propanol / 90% deionized water. Mix

well. Prepare fresh daily. (Nitrite is not stable over long periods

of time)

5.2.5.2 Standard 2: (0.1 ppm fluoride, 0.5 ppm acetate, 1.0

ppm formate, 0.4 ppm methanesulfonic acid (MSA), 1.0 ppm

chloride, 0.4 ppm nitrite, 1.0 ppm bromide, 0.4 ppm nitrate,

4.0 ppm adipate, 2.0 ppm succinate, 0.4 ppm sulfate, and

0.4 ppm phosphate) Pipet 1 ml of the combination stock stan-

dard solution to a 50 ml volumetric flask. Add 40 microliters of

1000 ppm nitrite purchased stock solution and dilute to vol-

ume with 10% 2-propanol / 90% deionized water. Mix well.

Prepare fresh daily. (Nitrite is not stable over long periods of

time).

5.2.5.3 Standard 3: (0.2 ppm fluoride, 1.0 ppm acetate, 2.0

ppm formate, 0.8 ppm methanesulfonic acid (MSA), 2.0 ppm

chloride, 0.8 ppm nitrite, 2.0 ppm bromide, 0.8 ppm nitrate,

8.0 ppm adipate, 4.0 ppm succinate, 0.8 ppm sulfate, and

0.8 ppm phosphate) Pipet 1 ml of the combination stock stan-

dard solution to a 25 ml volumetric flask. Add 80 microliters of

1000 ppm nitrite purchased stock solution and dilute to vol-

ume with 10% 2-propanol / 90% deionized water. Mix well.

Prepare fresh daily. (Nitrite is not stable over long periods of

time).

5.2.6 Prepare volumes of cation calibration standard solu-

tion for a three point calibration.

5.2.6.1 Standard 1: (0.05 ppm lithium, 0.5 ppm sodium,

ammonium, potassium, magnesium, and calcium) Pipet 1 ml

of the combination stock cation standard solution to a 100 ml

volumetric flask and dilute to volume with 10% 2-propanol /

90% deionized water and mix well. Prepare fresh daily.

5.2.6.2 Standard 2: (0.1 ppm lithium, 1.0 ppm sodium,

ammonium, potassium, magnesium, and calcium) Pipet 1 ml

of the combination stock standard solution to a 50 ml volu-

metric flask and dilute to volume with 10% 2-propanol / 90%

deionized water and mix well. Prepare fresh daily.

IPC-TM-650

Number

2.3.28.2

Subject

Bare Printed Board Cleanliness by Ion Chromatography

Date

12/2009

Revision

Page2of3