IPC-TM-650 EN 2022 试验方法.pdf - 第215页

1 Scope The purpose of this test method is to measure the amount of chlorine and bromine compounds in base materi- als. This test method is applicable to reinforced base materi- als with a minimum thickness of 0.3 mm [0.…

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.

age1of1

电子技术应用　　　　　　　ｗｗｗ．ＣｈｉｎａＡＥＴ．ｃｏｍ

1 Scope The purpose of this test method is to measure the

amount of chlorine and bromine compounds in base materi-

als. This test method is applicable to reinforced base materi-

als with a minimum thickness of 0.3 mm [0.012 in] and to

un-reinforced base materials with a minimum thickness of

0.08 mm [0.0031 in].

A combustion flask is used to extract ionic and covalent halo-

gen from the sample, and Ion Exchange Chromatography is

used for the quantitative analysis of halogen content.

2 Applicable Documents All terms and definitions in this

document conform to IPC-T-50,

Terms and Deﬁnitions for

Interconnecting and Packaging Electronic Circuitry.

The IPC Test Method is generated and written, verbatim, from

the IEC 61189-2 TEST 2C12: Total Halogen Content in

Base Materials.

3 Test Specimens Rigid or flexible base materials shall be

used for the test provided they meet the minimum thickness

requirements described in the scope. The copper foil (if appli-

cable) shall be removed from the test specimens by etching

by any industry acceptable etching method or by mechanical

peeling before test.

For reinforced base materials, the number of test specimens

shall not be less than five (5) with a minimum size of 1 cm x

1 cm [0.39 in x 0.39 in]. For unreinforced base materials, the

number of test specimens shall not be less than five (5) with a

minimum size of 1 cmx1cm[0.39 in x 0.39 in].

Wash the specimens thoroughly in distilled or deionized water.

For reinforced base materials, dry the sample at 105 °C [221

°F] +5/- 0 °C [+9 °F/-0 °F] for one hour + 0.25 hour /-0 hour.

For unreinforced base materials, wipe off the water with a lint-

free cloth or paper wiper and leave them to dry at room tem-

perature and atmospheric pressure for a minimum of one

hour.

4 Apparatus & Materials

a. Ion exchange chromatograph with a detection limit of 10

ppm or better.

b. Analytical balance with an accuracy of approximately 1

mg in weight or better.

c. Knife.

d. Tweezers.

e. Vinyl gloves.

f. Lint-free cloth, paper wipers or equivalent.

g. Quantitative filter paper.

h. Combustion flask, or equivalent.

i. Oxygen (99.9 % purity or better).

j. Gas pressure regulator.

k. Flint striker, or another ignition device.

l. Wash bottle.

m. Beaker.

n. Micro-pipette.

o. Flasks (various sizes).

p. Potentiometric titrator for silver nitrate, if necessary.

q. Platinum basket for holding sample.

r. Alkali solution.

s. Ethyl alcohol.

t. Chlorine ion standard solution for chromatograph.

u. Bromine ion standard solution for chromatograph.

v. Silver nitrate titrant, if potentiometric titration using silver

nitrate is used.

5 Procedure

5.1 Combustion Procedure

Weigh the specimen using

the analytical balance and record the result.

Place approximately 50 ml alkali solution in a combustion flask

to act as an absorbent of combustion gas.

Fill the combustion flask with oxygen.

Insert a test specimen into the combustion flask as shown in

Figure 1.

Insert a piece of filter paper into the combustion flask as

shown in Figure 1 to act as a fuse/flame starter.

Apply several drops of ethyl alcohol on the test specimen for

improving the ignition of the specimen and then ignite the

specimen.

3000 Lakeside Drive, Suite 309S

Bannockburn, IL 60015-1219

IPC-TM-650

TEST METHODS MANUAL

Number

2.3.41

Subject

Test Method for Total Halogen Content in Base

Materials

Date

04/06

Revision

Originating Task Group

Halogen Free Materials Subcommittee (4-33)

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.

Page1of3

ASSOCIATION CONNECTING

ELECTRONICS INDUSTRIES

Leave the flask at room temperature for 30 min ± 2 min after

combustion. The generated gas is absorbed into the alkali

solution to produce Cl

/Br

ion solution.

Transfer the solution from the combustion flask to a volumet-

ric flask. Introduce deionized water in the flask until the total

amount is 100 ml of the test solution.

Remove the suspended subjects from the test solution by fil-

tration or centrifugation if necessary.

Follow the same procedure outlined above without the test

specimen to prepare a reference test solution (blank) without

combustion of a test sample.

Note: Chlorine and bromine contents shall be measured

beforehand without any test specimen in the combustion

flask.

5.2 Chemical Analysis Inject the test fluid gathered from

the flask in 5.1 into the inlet of an ion exchange chromato-

graph shown in Figure 2.

Analyze the peak area/height of the Cl

/Br

conductivity on the

recorder and obtain Cl

/Br

concentration from a calibration

curve.

Obtain Cl

/Br

ion concentrations of the reference by compar-

ing its conductivity using the standard solution. The test

solution is compared to the reference solution (blank). Any

contaminant in the reference solution will be subtracted from

the test solution.

Titrate test solution using silver nitrate if concentration of Cl

ions is higher than 1 wt%. An example of analyzing condi-

tions for the ion exchange chromatography is given in Table 1.

IPC-2341-1

Figure 1 Absorb Combustion Gas Using a Combustion

Flask

Alkali solution

as absorbent

Platinum basket

(Test piece, filter

as fuse)

Fire

Combustion

flask (or

equivalents)

IPC-2341-2

Figure 2 Composition of Ion Exchange Chromatograph

Recorder

Waste

Fluid

Waste

Fluid

Conductivity

Detector

Suppressor

Separation

Column

Precolumn

Elimination Fluid

Delivering Pump

Elimination

Fluid

Inlet

Eluant

Delivering

Pump

Table 1 Example of Analyzing Conditions

for the Ion Exchange Chromatography

Item/Material Deﬁnition/Quantity

Eluant Alkali solution

Eluant delivering rate 1.0 ml/min to 2.0 ml/min

Elimination fluid H

Elimination fluid and delivering rate 1.0 ml/min to 2.0 ml/min

Column Precolumn,

separation column

Suppressor Suppression for anion

Detector Conductivity meter

IPC-TM-650

Number

2.3.41

Subject

Test Method for Total Halogen Content in Base Materials

Date

04/06

Revision

Page2of3