IPC-TM-650 EN 2022 试验方法.pdf - 第193页

5.2.6.3 Standard 3: (0.2 ppm lithium, 2.0 ppm sodium, ammonium, potassium, magnesium, and calcium) Pipet 1 ml of the combination stock standard solution to a 25 ml volu- metric flask and dilute to volume with 10% 2-propa…

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

5.2.6.3 Standard 3: (0.2 ppm lithium, 2.0 ppm sodium,

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

of the combination stock standard solution to a 25 ml volu-

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

deionized water and mix well. Prepare fresh daily.

5.2.7 Run a minimum 3 point calibration per the chromato-

graph manufacturer’s recommended methods for both anions

and cations, verifying correct standard concentrations have

been entered into the method.

5.2.8 Adjust the baselines and update the calibration as

required to obtain a good calibration curve. The correlation

factor (R

) for the curves should be a minimum of 0.98, with

higher values desirable. Any point on the calibration curve

should not deviate from the expected value by more than ±

10%.

Note: The organic acids standards will typically not form a lin-

ear calibration and a quadratic curve may be required.

5.3 Analytical Procedure

5.3.1

The analysis of the extract solution should be done as

soon as possible after extraction, but shall be no longer than

four days from the extraction date.

5.3.2 Start the chromatograph per the manufacturers rec-

ommended method and allow it to come to a stable baseline.

5.3.3 Analyze sample solutions for anion and cation content,

utilizing best analytical technique and laboratory practices.

5.4 Calculation of Results

5.4.1

Values from the chromatograms are typically reported

in parts per million (ppm).

5.4.2 Surface Area Calculation Record the surface area

of printed board (length x width x 2), e.g., a rectangular

printed board with no cutouts. Alternatively, the surface area

of the printed board can be determined from CAD software or

other machine vision recognition system. Surface area should

be known to three significant figures.

5.4.3 Results are to be expressed as micrograms (µg) of ion

per square centimeter based on the extraction volume and the

calculated sample surface area.

µg/cm

(SC − BL) x Vol

Area

where:

SC = ppm from IC (µg/mL)

BL = PPM from the bag blank

Vol = final volume (ml)

Area = surface area (cm

)

Note: ‘‘ppm’’ value is actually specimen value minus blank

value.

5.4.4 Report all ions quantified.

6 Notes

A repeatable and reproducible ionic cleanliness evaluation

method requires some level of skill in accurately running an ion

chromatography unit. The reader may find IPC-WP-008 to be

of use.

IPC-TM-650

Number

2.3.28.2

Subject

Bare Printed Board Cleanliness by Ion Chromatography

Date

12/2009

Revision

Page3of3

Scope

This

test method is used to measure pH in anhy-

drous fluorocarbon azeotropes and blends in cleaning and

defluxing equipment.

This method does not work in the presence of organic acid

acceptors normally present with chlorinated solvents, namely

1,1,1-trichloroethane and trichloroethylene.

Applicable Documents

None

Test Specimen

3.1

Approximately

25 ml samples of solvent are taken from

the boiling sump and condensate rinse sump of the operating

fluorocarbon vapor defluxer or degreaser and, for comparison

purposes, from the virgin solvent supply.

Equipment/Apparatus

4.1

indicator sticks TM ‘‘colorpHast’’® cat. #9590 avail-

able from MCB Manufacturing Chemists Inc., 2909 Highland

Ave., Cincinnati, OH 45212

4.2

Screw

cap glass vials (50 ml, three or six required per

test)

4.3

Graduated

glass cylinders (50 ml, three required per

test)

Caution: Plastic is sometimes attacked by solvents such as

acetone, methylene chloride azeotropes.

Procedure

5.1

Transfer

25 ml of virgin solvent to a clean vial using a

clean, dry graduated cylinder, insert a ‘‘colorpHast’’® plastic

strip, and cap the vial.

5.2

Repeat

5.1, sampling the defluxer or degreaser boiling

sump.

5.3

Repeat

5.1, sampling the condensate or rinse sumps.

5.4

Allow

the test vials to stand 30 minutes.

5.5

Compare

the colors on the test sticks with the ‘‘color-

pHast’’® color key and record the matching pH value.

5.6

Discard

the ‘‘colorpHast’’® indicator sticks and vials

after emptying the solvent into the boiling sump.

5.7

Rinse

the graduated cylinders with virgin solvent, empty

into the boiling sump, and allow to dry for reuse.

5.8

With

fluorocarbon/acetone and fluorocarbon/methylene

chloride azeotropes or mixtures, which attack the indicator

adhesive, repeat the above steps, but with two vials of each

sample. Cut the bottom two color squares off three ‘‘color-

pHast’’® sticks and discard the remainder of the stick. Put

one square of each color in samples from 5.1, 5.2, and 5.3

sources and complete steps 5.4 through 5.7.

5.9

Interpretation of Results

pH is above 5.5, this is an

acceptable condition. If pH is less than 5.5, the solvent is

contaminated by an accumulation of activated flux residues,

organic acids, or thermal degradation products of the solvent.

This requires inspection to establish the need for cleaning of

the equipment and for recovery of the solvent.

2215

Sanders Road

Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.30

Subject

Solvent

pH Determination in Anhydrous

Fluorocarbons Solvents

Date

11/81

Revision

Originating Task Group

N/A

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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