IPC-TM-650 EN 2022 试验方法.pdf - 第213页

5.2.3.2 Determination of F__film Prepare a film sample in a vial as standard. Make three injections with venting between injections and equilibration before each one, just as in the case of the liquid. The F__ret__film a…

5.1.2

Evaluation

The

volatile content of each specimen is

calculated as follows:

Volatile

Content (%)

−W

)(W

−W

)

−W

)

100

5.1.3

Report

The

results should be documented and con-

tain the following:

1. Certification that the test was performed in accordance

with this test method.

2. Identification of specimens tested.

3. Volatile content % for each specimen tested and the aver-

age.

Procedure

Method B

5.2 Calibration

5.2.1

Prepare

two liquid calibration mixtures as directed per

vendor instructions. The mixtures do not need to have these

exact amounts but the amount of each ingredient should be

measured precisely to within 0.0002 grams. The mixture

should be stored in a suitable container with a resealable

septa lid. Calibration mixtures should be appropriate for vola-

tiles present in product tested.

5.2.1.2

Make

sure the mixtures are each well mixed, then

determine the density of the mixtures by any acceptable

method.

5.2.1.3

From

each of the mixtures inject a minimum of four

different amounts (0.5 to 3.0 microliters each) into separate,

previously prepared, empty, sealed vials.

5.2.1.4

Allow

each vial to equilibriate in the headspace unit,

then inject each into the chromatograph and obtain an area

for each sample.

5.2.1.5

Plot

the areas vs. the amount (in milligrams) of each

ingredient. The eight points should all lie on the same straight

line.

5.2.1.6

Determine

the response factor Rf (milligrams/area

unit) for each ingredient. If the plot above is not linear or does

not pass through the origin, then it might be necessary to

have different Rf at different amounts.

5.2.2

Sample

5.2.2.1

Cut

and weigh a 25.4 mm square sample of mate-

rial to be tested. Place into sample vial and seal tightly. Equili-

brate sample in the headspace unit and then inject onto the

chromatography column. Allow the chromatogram to run for

eight minutes.

Note 1: Appropriate time and temperature dependent on

product tested.

5.2.2.2

Calculate

the amount of each calibrated peak using

the following equation.

Volatile % (i) = (Area (i) * Rf (i) * 100)/(Wt * F)

where: Area (i) = area generated for ith calibrated peak

Rf (i) = response factor for ith peak

Wa = weight of sample (not including substrate—

subtract out substrate weight by calculating

the area x the density of the substrate under

test (W

)

and subtracting the value from the

total sample weight (Wt). Wt −Ws = Wa)

F = fraction of ingredient in film that reaches the

chromatography relative to the same frac-

tion of pure liquid.

5.2.3

Determination of F

5.2.3.1 Determination of F__liq

Prepare

a mixture of

ingredients to be tested. Inject 1 to 2 microliters of the mixture

into a sealed vial. Equilibrate in the head space unit, then

inject into the chromatograph and obtain the area for each

peak of interest.

5.2.3.1.1

Immediately

after the injection is complete, vent

the vial by means of a small syringe needle and replace the

vial to allow it to equilibrate again. Again after equilibration

inject the vial into the chromatograph.

5.2.3.1.2

Vent

the vial a second time and equilibrate and

inject again. There should have been three injections, each

preceded by an equilibration and two ventings, one immedi-

ately after the first injection and the other immediately after the

second injection.

5.2.3.1.3

Calculate

F__ret__liq and F__liq for each ingredi-

ent as follows.

F__ret__liq = (square root (area3/area2) + area2/area1)/2

F__liq = 1 − F__ret__liq

IPC-TM-650

Number

2.3.37

Subject

Volatile

Content of Adhesive Coated Dielectric Films

Date

5/98

Revision

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5.2.3.2

Determination of F__film

Prepare

a film sample in

a vial as standard. Make three injections with venting between

injections and equilibration before each one, just as in the

case of the liquid. The F__ret__film and F__film are calculated

in exactly the same way as F__ret__liq and F__film, except

that the areas used are generated by the film sample.

5.2.3.3

F__liq

and F__film are determined at least eight

times, preferably over a period of several days. Approximately

the same number of liquids as films are tested each day. The

values of F__liq and F__film are averaged separately.

5.2.3.5

Once

determined, F should not change unless the

ingredients change or unless the equilibrium conditions

change.

5.2.3.6

Different

materials will have different values of F.

6 Notes

Multiple

Headspace Extraction—A Procedure for Quantita-

tive Analysis of Volatile Compounds in Solid Samples

Kolb,

Auer, and Pospisil, ANGEWANTE CHROMATOGRAPHIE—

APPLIED CHROMATOGRAPHY, January, 1981.

IPC-TM-650

Number

2.3.37

Subject

Volatile

Content of Adhesive Coated Dielectric Films

Date

5/98

Revision

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1.0

Scope

This

test method establishes a procedure for

determining the thermal decomposition temperature of

organic films using thermogravimetric analysis (TGA).

2.0

Applicable Documents

ASTM D 618

Standard

Practice for Conditioning Plastics and

Electrical Insulating Materials for Testing

ASTM

D 3850

Standard

Test Method for Rapid Thermal

Degradation of Solid Electrical Insulating Materials by Thermo-

gravimetric Analysis

3.0

Test Specimen

The

free films are cut to fit into the

TGA sample pan giving an initial weight of nominally 2-20 mg.

4.0

Apparatus or Material

Thermal

gravimetric analysis

equipment equipped with air, nitrogen purge, capable of

maintaining 5°C heating rate from ambient to 800°C, such as

TA Instruments or Perkin Elmer TGA instruments.

5.0

Procedure

5.1

The

test specimens should be conditioned at 23 ± 2°C

and 50 ± 5% relative humidity for not less than 24 hours prior

to testing. Refer to ASTM D 618 and ASTM D 3850.

5.2

the manufacturer’s recommendations for equip-

ment startup and calibration.

5.3

Set

the dry nitrogen purge rate at 55 cc/min.

5.4

Allow

the instrument to purge for 30 min.

5.5

Heat

at a rate of 5°C/min from ambient to 150°C.

5.6

Hold

the temperature for 15 min to remove any moisture

from the specimen.

5.7

Heat

at a rate of 5°C/min to 800°C.

5.8

Record

the temperature at which 5% additional weight

loss occurs based on the weight after the 150°C hold.

5.9 Repeat

steps 5.3-5.6 with dry air instead of nitrogen

using a new sample.

5.10

Report

the thermal decomposition temperature, T

max

degrees Celsius (°C), followed by the evaluation criteria

(e.g., 5% wt. loss), and the atmosphere under which the test

was conducted (e.g., nitrogen), e.g. 185°C (5% wt. loss, nitro-

gen).

6.0

Notes

6.1

Calibration

of the instrument must be carried out

according to the manufacturer’s recommendations. The rate

of flow of the gas in the cell will have a significant effect on the

calibration, therefore the instrument must be calibrated with

the same flow rate used during the test. After the instrument

has been calibrated, the flow rate should not be changed.

6.2

The

surface area of the test specimen will affect the

results. If two specimens of the same material are tested, one

with a large surface area and one with a small surface area,

both of the same mass, the specimen with the smaller surface

area will normally lose weight at a slower rate.

6.3

The

specimen may initially gain weight due to buoyancy

effects.

The

Institute for Interconnecting and Packaging Electronic Circuits

2215 Sanders Road • Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.40

Subject

Thermal

Stability

Date

7/95

Revision

Originating Task Group

Deposited Dielectric Task Group (C-13a)

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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