IPC-TM-650 EN 2022 试验方法.pdf - 第209页

5.2.2.3 Dilute solution to exactly 1 liter and stopper. See 6.3 for safety and handling information and 6.4 for first aid infor- mation. 5.3 Test Procedure 5.3.1 Measure specific gravity of sample using ASTM Method D 211…

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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5.2.2.3

Dilute

solution to exactly 1 liter and stopper. See 6.3

for safety and handling information and 6.4 for first aid infor-

mation.

5.3

Test Procedure

5.3.1

Measure specific gravity of sample using ASTM

Method D 2111-95.

5.3.2

Bulb

pipet exactly 25 ml sample into a 250 ml Erlen-

meyer flask.

5.3.3 Bulb

pipet exactly 25 ml hydrochlorination reagent into

sample, stopper, then mix thoroughly.

5.3.4

Let

sit 15 to 20 minutes for complete reaction. During

reaction time, a blank may be run (see 5.3).

5.3.5

When

reaction time is complete, add five drops of bro-

mothymol blue 0.1% solution with an eye dropper.

5.3.6

Titrate

the sample to endpoint with 0.1 N NaOH solu-

tion. The endpoint is reached when solution color changes

from yellow to blue.

5.4

Blank

5.4.1

Bulb

pipet exactly 25 ml hydrochlorination reagent into

a 250 ml Erlenmeyer flask.

5.4.2

Add

five drops bromothymol blue 0.1% solution with

an eye dropper.

5.4.3

Titrate

blank to endpoint with 0.1 N NaOH solution.

The endpoint is reached when solution color changes from

yellow to blue.

5.5

Disposal of Solutions

5.5.1 0.1 N NaOH in Methanol, Unused

This

solution is

dilute and readily soluble in water, hence it can be safely

poured down the sink. Flush with excess water.

5.5.2

All Other Solutions

NOT POUR DOWN THE

SINK. Place the solutions in appropriate, labeled, metal con-

tainers to be buried or burned in accordance with local, state,

and federal regulations.

5.6

Cleaning Glassware

Use

soap and water to clean any

glassware. Rinse well with excess water.

5.7

Safety and Handling, First Aid

See

6.3 and 6.4.

6 Notes

6.1

Calculations:

(B−A) x 0.4

sample x specific gravity (1)

= Total Acid Acceptance as % of NaOH

where:

= ml of 0.1 N NaOH used to titrate sample

B = ml of 0.1 N NaOH used to titrate blank

(1)

See sale specification for specific gravity of solvent choice.

6.2

Interpreting Test Results*

Chlorinated

Solvent

Methylene

Chloride

1,1,1-

Trichloroethane

Perchloroethylene

Within Normal

Range

>0.08%

>0.04%

Solvent is Borderline

Check Daily

0.04%-0.08%

≤0.04%

A) Discard

B) Remove, distill blend

with virgin solvent at 4

parts virgin solvent, 1

part distilled.

<0.04%

*Note: These

guidelines have been established using inhibited chlorinated solvents from the

Dow Chemical Company. The solvent manufacturer should be consulted for particular inter-

pretation.

6.3

Safety and Handling

6.3.1 Sampling Procedure

Wear

safety goggles and neo-

prene or neoprene-coated gloves. Have adequate ventilation.

Avoid sparks or flames.

6.3.2

Laboratory Procedure

There

are no unusual haz-

ards inherent in this method, but good ventilation and normal

laboratory safety precautions should be employed. When pre-

paring reagents, mixing should be employed in a hood and

chemical goggles should be worn. Keep away from any

sparks or flames.

IPC-TM-650

Number

2.3.36

Subject

Acid

Acceptance of Chlorinated Solvents

Date

10/85

Revision

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0SHA

recommended exposure limits for chlorinated sol-

vents (all in parts per million).

Chlorinated

Solvent

Perchloroethylene

Trichloroethylene

1,1,1-Trichloroethane

Methylene

Chloride

OSHA

8Hr

TWA

100

350

500

ACGIH

TLV

350

100

ACC

200

450

1000

AMP

300/5 min. in any 3 hrs.

200/5 min. in any 2 hrs.

2000/5 min. in any 2 hrs.

a. No limits established by OSHA. ACGIH recommends a short term exposure limit (STEL) of

450 ppm.

(1) TWA–Time Weighted Average

(2) ACGIH–American Conference of Governmental Hygienists

TLV–Threshold limit values from ACGIH Handbook, 83/84

(3) ACC–Acceptable Ceiling Concentration

(4) AMP–Acceptable Maximum Peak

6.4

First Aid

6.4.1 Eye Contact

Rinse

eyes with running water for at

least 30 minutes. Prompt medical attention is essential.

6.4.2

Skin Contact

Flush

the area thoroughly with water.

Wash clothing before reusing it.

6.4.3

Oral Ingestion

NOT INDUCE VOMITING. Call a

physician or transport the worker to an emergency facility.

6.4.4

Inhalation

Remove

the worker to fresh air if the

worker starts feeling dizzy or light-headed. Contact a physi-

cian or transport the worker to a medical facility. If breathing

stops, give mouth-to-mouth resuscitation. Administer oxygen

when breathing starts (see 6.3.2 for chlorinated solvent expo-

sure limits).

6.4.5

Additional Help

For

any additional chemical related

medical help, call Chemtree Emergency at 800) 424-9000. In

Canada call (collect) Canutel (613) 996-6666.

6.5

All

equipment and chemicals used were purchased from

Van Waters and Rogers standard lab supply catalog.

6.6

This

test is designed for the base chlorocarbons only;

therefore, discretion should be used when testing bipolar sol-

vents.

6.7

Specific Questions

Any

specific questions can be

referred to Dow Chemical U.S.A., Inorganic Chemicals

Department, Technical Service and Development, Midland,

Mich. 48640.

IPC-TM-650

Number

2.3.36

Subject

Acid

Acceptance of Chlorinated Solvents

Date

10/85

Revision

age3of3

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