IPC-TM-650 EN 2022 试验方法.pdf - 第143页

1 Scope This test method specifies two methods for the determination of the acid value of a flux of type L, M or H. Method A is a potentiometric titration method and is to be considered the reference method. Method B is …

able 1

Cloth

No.

Nominal

idth

Inches

Thickness

Inch

Weight

Per

Square

Yard

Ounces

Yarn,

Warp,

and Fill Construction

Minimum

Breaking

Strength Per

Inch of Width

Yards per

Standard

Roll Type of Weave

Warp

Pounds

Fill

Pounds

106

38 0.0015 0.85 900-1/0 56x56 46 52 250 ± 25 Plain

108 38 0.0020 1.43 900-1/2 60x47 70 40 250 ± 25 Plain

112 38 0.0030 2.09 450-1/2 40x39 82 80 250 ± 25 Plain

113 38 0.0030 2.46 450-1/2

900-1/2

60x64 123 60 250 ± 25 Plain

116 38 0.0040 3.16 450-1/2 60x58 123 120 250 ± 25 Plain

119 38 0.0040 2.80 450-1/2 54x50 110 100 250 ± 25 Plain

120 38 0.0040 3.16 450-1/2 60x58 125 120 250 ± 25 4-harness satin

126-150 38 0.0060 5.50 150-1/2 34x32 225 195 250 ± 25 Plain

126 38 0.0065 5.37 450-3/2 34x32 205 185 250 ± 25 Plain

127 38 0.0070 6.00 450-3/2 42x32 225 185 250 ± 25 Plain

128 38 0.0070 6.00 225-1/3 42x32 250 200 250 ± 25 Plain

128-150 38 0.0067 6.00 150-1/2 42x32 250 200 250 ± 25 Plain

140 38 0.0100 8.70 450-4/3 32x21 400 290 125 ± 25 Plain

141 38 0.0100 8.70 225-2/3 32x21 400 290 125 ± 25 Plain

143 38 0.0090 8.90 225-3/2

450-1/2

49x30 611 56 125 ± 25 4-harness satin

143-150 38 0.0086 9.40 150-2/2

450-1/2

49x30 660 70 125 ± 25 4-harness satin

148 38 0.0120 10.10 450-3/5 30x19 450 360 125 ± 25 Plain

149 38 0.0120 10.80 225-2/4 30x19 450 360 125 ± 25 Plain

161 38 0.0150 12.20 450-4/5 28x16 550 450 125 ± 25 Plain

162 38 0.0150 12.20 225-2/5 28x16 450 350 125 ± 25 Plain

164 38 0.0150 12.60 225-4/3 20x18 500 450 125 ± 25 Plain

164-150 38 0.0140 13.00 150-4/2 20x18 500 450 125 ± 25 Plain

181 38 0.0085 8.90 225-1/3 57x54 340 330 125 ± 25 8-harness satin

181-150 38 0.0080 9.50 150-1/2 56x54 350 325 125 ± 25 Plain

182 38 0.0130 12.40 225-2/2 60x56 440 400 125 ± 25 8-harness satin

182-150 38 0.0134 12.65 150-1/3 60x56 440 400 125 ± 25 Plain

183 38 0.0180 16.75 225-3/2 54x48 650 620 75 ± 15 8-harness satin

184 38 0.0270 25.90 225-4/3 42x36 950 800 50 ± 10 8-harness satin

184-150 38 0.0246 24.16 150-4/2 44x35 950 800 50 ± 10

573-150 38 0.0110 8.00 150-3/2 16x16 335 316 125 ± 25 Plain

1000-150 38

and

0.0130 9.66 150-4/2 16x14 450 410 125 ± 25 Plain

1044-150 38 0.0220 19.20 ...... 16x14 450 410 125 ± 25 Plain

1523-150 38 0.0140 11.70 150-3/2 28x20 525 400 125 ± 25 Plain

1527-150 38 0.0150 12.90 150-3/3 17x17 535 485 125 ± 25 Plain

IPC-TM-650

Number

2.3.11

Subject

Glass

Fabric Construction

Date

4/73

Revision

age3of3

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Scope

This

test method specifies two methods for the

determination of the acid value of a flux of type L, M or H.

Method A is a potentiometric titration method and is to be

considered the reference method.

Method B is an alternative, visual end-point, titration method.

Applicable Documents

ISO 9455

Soft

Soldering Fluxes, Test Methods

IPC-TM-650

Test

Methods Manual

2.3.34 Solids Content, Flux

IPC

J-STD-004

Requirements

for Soldering Fluxes

Test Specimen

minimum of 2.0 grams of liquid flux, 10

grams of solder paste, 150 grams of cored wire or 10 grams

of solder preforms.

Apparatus and Reagents

4.1 General

4.1.1

Use

only reagents of recognized analytical quality and

only deionized water.

4.1.2

Ordinary

laboratory apparatus.

4.2

For Potentiometric Titration Method (Method A)

4.2.1

Tetrabutyl

ammonium hydroxide, 0.1 M (0.1 mole/L).

Use a commercially available standard solution or one pre-

pared from a commercially available concentrated standard

solution by dilution with 2-propanol (4.2.2). Alternatively, pre-

pare a 0.1 M tetrabutyl ammonium hydroxide solution by dilut-

ing a commercial concentrated solution with 2-propanol and

standardize this solution against an accurately weighed

amount of benzoic acid (about 0.5 g) dissolved in dimethylfor-

mamide, previously neutralized to thymol blue.

4.2.2

2-Propanol.

Neutralized with tetrabutyl ammonium

hydroxide solution (4.2.1) to a faint pink color using phenol-

phthalein as an indicator.

4.2.3

Ethanol,

anhydrous. Neutralized with tetrabutyl ammo-

nium hydroxide solution (4.2.1) to a faint pink color using phe-

nolphthalein as an indicator.

4.2.4 Toluene.

Neutralized with tetrabutyl ammonium

hydroxide solution (4.2.1) to a faint pink color using phenol-

phthalein as an indicator.

4.2.5

Ethanol/toluene

mixture. Mix equal volumes of the

neutralized anhydrous ethanol (4.2.3) and neutralized toluene

(4.2.4).

4.2.6

Phenolphthalein

Indicator.

4.2.7 Millivoltmeter

or pH meter.

4.2.8

Glass

electrode.

4.2.9

Saturated

calomel, or silver chloride/silver, electrode.

4.2.10

Magnetic

or mechanical stirrer with variable speed

drive.

4.2.11 Burette

capable of delivering aliquots of 0.1 ml to 1.0

ml.

4.3

For Titration with Visual End-Point (Method B)

4.3.1

Ethanol,

anhydrous. Neutralized with potassium

hydroxide, 0.1 M in alcohol (4.3.5), to a faint pink color using

phenolphthalein as an indicator.

4.3.2

Toluene.

Neutralized with potassium hydroxide, 0.1 M

in alcohol (4.3.5), to a faint pink color using phenolphthalein as

an indicator.

4.3.3

Ethanol/toluene

mixture. Mix equal volumes of the

neutralized anhydrous ethanol (4.3.1) and neutralized toluene

(4.3.2).

4.3.4 2-Propanol.

Neutralized with potassium hydroxide, 0.1

M in alcohol (4.3.5), to a faint pink color using phenolphthalein

as an indicator.

2215

Sanders Road

Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.13

Subject

Determination

of Acid Value of Liquid Solder Flux -

Potentiometric and Visual Titration Methods

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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4.3.5

Potassium

hydroxide solution, 0.1 M in alcohol. Use a

commercially available standard solution or one prepared from

a commercially available concentrated standard solution by

dilution with ethanol (4.3.1). Alternatively, prepare an approxi-

mate 0.1 M potassium hydroxide solution by dissolving 3 ±

0.1 g potassium hydroxide (KOH) in 500 ml of ethanol (4.3.1),

and standardize this solution against an accurately weighed

amount of benzoic acid (about 0.5 g) dissolved in ethanol

(4.3.1).

4.3.6

Phenolphthalein

indicator solution. Add 1g of phenol-

phthalein to approximately 50 ml methanol and mix. When

dissolved, dilute to 100 ml with methanol and mix.

Procedures

5.1 Potentiometric Titration (Method A)

5.1.1

preliminary experiments, determine whether the

sample is soluble in 2-propanol, anhydrous ethanol, toluene or

the ethanol/toluene mixture. If the sample is not completely

soluble in any of these solvents, select the one in which the

sample appears to be the most soluble. If the sample is

equally soluble in all four solvents, then use neutralized

2-propanol (4.2.2).

5.1.2

Carry

out the following procedure, in triplicate, on the

flux sample.

5.1.2.1

Weigh, to the nearest 0.001 g, 2 to5goftheliquid

flux sample, taking steps to prevent loss of volatile matter

during the weighing. The larger size (≈5 g) sample is required

for very low solids fluxes. Transfer the weighed sample to a

250 ml low form beaker.

5.1.2.2 Dilute

the sample to 100 ml with 2-propanol (4.2.2),

or the selected solvent (4.2.3 to 4.2.5), according to the solu-

bility characteristics of the flux. Cover with a watch glass and

dissolve the flux by gentle agitation.

5.1.2.3

Place

the beaker on the stand of the titration assem-

bly with the electrodes, stirrer and burette in position. Adjust

the speed of the stirrer to give vigorous stirring without splash-

ing. Titrate with the 0.1 M tetrabutyl ammonium hydroxide

solution (4.2.1), adding 1.0 ml portions and recording the pH

or mV meter reading after each addition. As the end-point is

approached, reduce the additions of titrant to 0.1 ml and con-

tinue titrating past the end-point.

5.1.2.4

Plot

the pH or potential values against the volume of

titrant added to obtain the titration curve. The point of inflec-

tion of the curve corresponds to the end-point of the titration.

Note: The point of inflection of the curve may conveniently be

determined by using the derivative curve.

5.1.2.5

Carry out a blank determination, using reagents

only, for comparison purposes.

5.2

Visual Titration (Method B)

5.2.1

preliminary experiments, determine whether the

sample is soluble in 2-propanol, anhydrous ethanol, toluene or

the ethanol/toluene mixture. If the sample is not completely

soluble in any of these solvents, select the one in which the

sample appears to be the most soluble. If the sample is

equally soluble in all four solvents, then use neutralized etha-

nol (4.3.1) as the selected solvent.

5.2.2

Carry

out the following procedure, in triplicate, on the

flux sample.

5.2.2.1

Weigh,

to the nearest 0.001 g, sufficient flux sample

to correspond to approximately1gofnonvolatile matter (see

IPC-TM-650, Test Method 2.3.34), taking steps in the case of

liquid flux samples to prevent loss of volatile matter during the

weighing.

5.2.2.2

Transfer

the weighed sample to a suitable flask or

beaker and add 100 ml of the selected solvent. Stir until the

sample has dissolved as completely as possible. Do not heat.

5.2.2.3

Add

three drops of phenolphthalein indicator solu-

tion (4.3.6) and titrate with the 0.1 M potassium hydroxide

solution (4.3.5) until a faint pink color persists throughout the

titrated solution for 15 seconds.

5.2.2.4

Carry

out a blank determination, using reagents

only, for comparison purposes.

5.3

Calculation of Results

The

acid value is expressed in

milligrams of potassium hydroxide per gram of nonvolatile

matter, regardless of the alkali used to perform the titration.

5.3.1

The

acid value (expressed in milligrams of potassium

hydroxide per gram of nonvolatile matter) is given by:

56.11VM

IPC-TM-650

Number

2.3.13

Subject

Determination

of Acid Value of Liquid Solder Flux -

Potentiometric and Visual Titration Methods

Date

06/04

Revision

age2of3

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