IPC-TM-650 EN 2022 试验方法.pdf - 第207页

6.1.4 If glassware is used during testing, it is recommended that it should be cleaned thoroughly prior to use to eliminate the possibility of interfering contaminants. 6.2 Safety Observe all appropriate precautions on M…

ppm

Fluoride Sample ml Chloroform ml

0.1-1.0

25 25

1.0-10.0 5 5

5.2.2

Tare

a beaker and add sample. Record the weight of

the flux to 0.001 gram.

5.2.3

Add

chloroform and 50 ml DI water and mix with stir-

rer for 10 minutes. Stop mixing and allow to stand for five

minutes.

5.2.4

Carefully

decant the water solution through filter paper

in funnel into a clean beaker. Allow sample to drain com-

pletely.

5.3

Standard Solutions

5.3.1

ppm fluoride (0.001%) – This standard can be pur-

chased ready-to-use. Alternately, a solution can be prepared.

Weigh 0.0221 gram reagent grade NaF (dried to 140 °C

[284 °F]). Add 500 ml DI water. Dilute to one liter in a volumet-

ric flask with total ionic strength adjustment buffer (TISAB).

5.3.2 1.0

ppm fluoride (0.0001%) – This standard can be

purchased ready-to-use. Alternately, a solution can be pre-

pared. Weigh 0.0023 gram reagent grade NaF (dried to

140 °C [284 °F]). Add 500 ml DI water. Dilute to one liter in a

volumetric flask with TISAB.

5.3.2.1

Another

method is to dilute 100 ml of 10 ppm fluo-

ride standard with 450 ml DI water and dilute to one liter in a

volumetric flask with TISAB.

5.3.3

0.1

ppm fluoride (0.00001%) – This standard is pre-

pared by diluting 100 ml of 1.0 ppm fluoride standard with

450 ml DI water and diluting to one liter in a volumetric flask

with TISAB.

5.3.3.1

Another

method is to dilute 10 ml of 10 ppm fluoride

standard with 495 ml DI water and dilute to one liter in a volu-

metric flask with TISAB.

5.4

Double Reference Electrode Filling Solutions

Inner

chamber filling solution saturated with AgCl.

Outer chamber filling solution filled with 10% KNO

5.5

Test

For

accurate results, allow all samples and stan-

dards to reach the same temperature before attempting a

measurement. Stir the samples and standards while a mea-

surement is being made.

5.5.1

Prepare

two standards that differ in concentration by

a factor of 10. The standards should bracket the expected

sample concentration.

5.3.2

Dilute

50 ml of the two standard solutions, each with

50 ml of DI water.

5.5.3

While

stirring with a magnetic stirrer, immerse elec-

trodes in the more dilute standard solution.

5.5.4

Remove

and rinse electrodes with DI water. Immerse

electrodes in the more concentrated standard solution.

5.5.5

the sample prepared per instructions for water

soluble flux, add 25 ml TISAB. While stirring, immerse elec-

trodes. Record indicated value.

5.6

Evaluation

The

fluoride value is typically displayed in

parts per million (ppm) fluoride. To obtain fluoride as weight

percentage of the nonvolatile content, use the following for-

mula:

Fluoride % of Solids =

(MS)100

Where:

is indicated value in ppm

M is mass of the flux sample in grams

S is the percentage of solids (nonvolatile chemicals) in the flux

sample

Notes

6.1 Standardization and Limits

Restandardization

should

be done every few hours or as recommended by the equip-

ment manufacturer to compensate for electrode drift.

6.1.1

Reproducibility is typically ± 2% obtainable with hourly

recalibration. Temperature fluctuation, drift and noise will limit

reproducibility.

6.1.2

Detection

limits are 0.02 ppm minimum and no known

maximum. A list of possible interfering ions has not yet been

determined for this electrode method.

6.1.3

Using

the same batch of DI water for dilutions will

eliminate the need to run blanks.

IPC-TM-650

Number

2.3.35.2

Subject

Fluoride

Concentration, Fluxes-Quantitative

Date

06/04

Revision

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6.1.4

glassware is used during testing, it is recommended

that it should be cleaned thoroughly prior to use to eliminate

the possibility of interfering contaminants.

6.2

Safety

Observe

all appropriate precautions on MSDS

for chemicals involved in this test method.

IPC-TM-650

Number

2.3.35.2

Subject

Fluoride

Concentration, Fluxes-Quantitative

Date

06/04

Revision

age3of3

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Scope

This

test is a method for determining acid accep-

tance of chlorinated solvents.

Acid acceptance is applicable for evaluating the condition of

the following inhibited chlorinated solvents.

• Perchloroethylene

• 1,1,1-Trichloroethane

• Methylene Chloride

• Trichloroethylene

Applicable Documents

ASTM D2111-95

Standard

Test Methods for Specific Gravity

of Halogenated Organic Solvents and Their Admixtures

Test Specimen

3.1

ml of solvent (see 5.1 for sampling procedure)

Apparatus

4.1

One

flask, Erlenmeyer, 100 ml, with glass stoppers (see

6.5)

4.2

Two

flasks, Erlenmeyer, 250 ml, with glass stoppers (see

6.5)

4.3

Two

flasks, Volumetric, 1000 ml, with glass stoppers

(see 6.5)

4.4

Two

pipets, 25 ml, with bulb (see 6.5)

4.5

One

pipet, graduated (calibrated), with bulb (see 6.5)

4.6 One

eye dropper (see 6.5)

4.7

One

balance, analytical (see 6.5)

4.8

Two

pieces of weighing paper (see 6.5)

4.9

Sodium

hydroxide 0.1 N in C.P. anhydrous methanol

(5.2.1 & 6.5)

4.10

Hydrochlorination

reagent, 0.1 N Hydrochloric acid in

anhydrous isopropanol (see 5.2.2 & 6.5)

4.11

Bromothymol

blue indicator, 0.1% solution

Note: Make sure all glassware is clean and dry.

Procedure

5.1 Sampling Procedure

5.1.1

Securely

tie a copper wire around the neck of a 100 ml

Erlenmeyer flask. Carefully lower, allow to fill, stopper, and

store in cool, dark place.

5.1.2

Since

a representative sample is desired, sampling

should be done when the tank is half full. Most tanks (or hoses

from them) have sampling points. From here, fill a 100 ml

Erlenmeyer flask, stopper, and store in a cool, dark place.

5.1.3

See

6.3 for safety and handling and 6.4 for first aid.

5.2

Reagent Preparation

5.2.1 Sodium Hydroxide Solution Preparation

5.2.1.1

Weigh

4.0 g reagent grade NaOH.

5.2.1.2

Pour

approximately 500 ml C.P. anhydrous metha-

nol into a 1 liter volumetric flask.

5.2.1.3

Add

NaOH and swirl until dissolved.

5.2.1.4

Dilute

solution to exactly 1 liter with methanol and

stopper. See 6.3 for safety and handling information and 6.4

for first aid information.

5.2.2

Hydrochlorination Reagent Preparation

5.2.2.1

Pour

about 500 ml anhydrous isopropanol into an 1

liter volumetric flask.

5.2.2.2

Bulb

pipet exactly 8.50 ml 37% HCl into the flask,

then swirl.

The

Institute for Interconnecting and Packaging Electronic Circuits

2215 Sanders Road • Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.36

Subject

Acid

Acceptance of Chlorinated Solvents

Date

10/85

Revision

Originating Task Group

N/A

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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