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SEMI G29-1296 E © SEMI 1986, 2002 1 SEMI G29-1296 E TEST METHOD FOR TRACE CO NTAMINANTS IN MOLDING COMPOUNDS E This document was editorially modifi ed in September 2002. Changes were made to Section 5.4 to correct a typo…

SEMI G28-0997 © SEMI 1986, 1997 8

Figure 8

S.O. Leadframe

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SEMI G29-1296

TEST METHOD FOR TRACE CONTAMINANTS IN MOLDING

COMPOUNDS

This document was editorially modified in September 2002. Changes were made to Section 5.4 to correct a

typographical error.

1 Purpose

1.1 This specification defines the test method for

determination of extractable trace contaminants in

molding compound.

2 Scope

2.1 This test method is suitable for all molding

compound materials and may be used by supplier and

customers to determine the trace contaminants in

molding compound.

2.2 This standard does not purport to address safety

issues, if any, associated with its use. It is the

responsibility of the users of this standard to establish

appropriate safety health practices and determine the

applicability or regulatory limitations prior to use.

3 Referenced Documents

3.1 ASTM Documents

ASTM D 1193 — Specification for Reagent Water

ASTM D 4327 — Anions in Water by Ion

Chromatography

4 Method Summary

4.1 Plastic molding compound material is molded,

ground to a defined mesh size, and placed into a sealed

extraction vessel with de-ionized water. Extraction is

carried out at 120 ± 2° C for 48 hours. The extract is

analyzed for both anionic and cationic impurities.

5 Sample Preparation

5.1 Samples of molding compound materials may be

obtained from either standard molding operations, or

prepared in the laboratory.

5.1.1 Samples from molding operations may include

mold runners post-cured according to manufacturer’s

recommendations.

5.1.2 To secure a sample in the laboratory, spread a

thin layer of uncured compound in a dedicated clean

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohocken, Pennsylvania 19428-2959, USA.

Telephone: 610.832.9585, Fax: 610.832.9555 Website:

www.astm.org

teflon-coated container. Cure and post-cure the

compound material according to manufacturer’s

recommendations.

5.2 Crush the cured material using a suitable grinding

apparatus, such as Spex mixer-mill No. 8000, or

equivalent.

NOTE 1: The grinder used must not generate excess localized

heat, or else sample decomposition and erroneous results may

be generated.

NOTE 2: Addition of liquid nitrogen is a suitable method for

eliminating undesirable thermal decomposition during

grinding.

5.3 Remove the ground compound and sieve it. Collect

for analysis the portion which passes through a 40 mesh

size, but is retained on a 100 mesh size screen. This

particle size is best suited for adequate extraction of

impurities.

5.4 Weigh 10 ± 0.1 grams of the powdered material

and place in an extraction vessel. Parr bombs with

teflon liners are suitable extraction vessels. Add 100 ml

de-ionized water. Prepare blank extraction vessel by

processing it in the same manner as your sample.

Weigh the sealed bombs and record their weights. Place

the sealed bottles on their sides in an oven at 120 ± 2° C

for forty-eight (48) hours.

NOTE 3: Certain compounds may require addition of reagent

grade methanol 10% (V:V) to enhance wetting.

5.5 At the completion of forty-eight (48) hours of

extraction, allow the bombs to cool to room

temperature and reweigh. If the weight loss exceeds 0.5

grams the sample should not be used for analysis.

Portion of this extract may be used to generate pH and

conductivity data. Anion analysis may be performed

using ion chromatography or specific ion electrodes.

Cation analysis may be conducted using atomic

absorption, plasma spectrometry, or ion

chromatography.

NOTE 4: It is important to avoid contamination with

particulate matter in the extract used for the analysis by AA,

ICAP, or IC. This procedure addresses determination of

extractive species only.

SEMI G29-1296

6 Instrumentation Techniques

6.1 Measurement of Conductivity

6.1.1 Apparatus — Conductivity Meter Model RC1682

with microconductivity cell, industrial instruments, or

equivalent.

6.1.2 Measurement — Measure conductivity of the

sample and black solutions. Calculate the specific

conductance of sample using the following equation:

= (L

- L

) K

- Specific conductance, S cm

-1

- Conductance of extract, S

- Conductance of the blank

K - Conductivity cell constant

6.2 Measurement of pH

6.2.1 Apparatus

6.2.1.1 pH meter (Orion, Model 601, or equivalent)

6.2.1.2 pH standard solutions

6.2.2 Measurement — Adjust pH meter indicator by

using standard solutions. Remove the electrodes with

de-ionized water and dry with clean filter paper. Place

the electrodes into the molding compound extract.

Allow the meter to equilibrate. Record the pH value.

6.3 Ion Specific Electrodes — Ion-specific electrodes

may be used for the determination of chloride, bromide,

sulfate, and phosphate. A separate specific electrode for

each ion is required and, in some instances, a reference

electrode may be necessary to complete the test.

Individual standards are needed for each ion tested.

Methodology recommended by the manufacturer for

each ion specific electrode should be closely followed.

Measured concentrations corrected for blank value

should be compared to the known standards in the

range 0.1–100 ppm. Chloride and bromide are usually

determined, using a solid state single electrode.

Determination of sulfate and phosphate ions may

require use of additional buffers and a titration.

6.4 Determination of Sodium, Potassium, and

Antimony Using Atomic Absorption

6.4.1 Apparatus — Atomic absorption

spectrophotometer.

6.4.2 Standard Solutions

6.4.2.1 Sodium standard solutions 0.1, 0.2, 0.4, 0.6,

0.8, 1.0 ppm.

6.4.2.2 Potassium standard solutions 0.1, 0.2, 0.4, 0.6,

0.8, 1.0 ppm.

6.4.2.3 Antimony standard solution 0.1, 0.2, 0.4, 0.6,

0.8, 1.0 ppm.

6.4.3 Measurement — Set up instrument according to

manufacturer’s recommendation. Analyze water extract

based on the calibration curve prepared using standard

solutions to obtain concentration of ion of interest.

6.4.4 Calculation

6.5 Determination of Chloride, Bromide, Phosphate,

Sulfate, Sodium, and Potassium by Ion

Chromatography

6.5.1 Method Principle — Ion chromatography is a

form of liquid chromatography used in the separation

and quantitation of ions. A filtered aliquot of sample is

injected into an Ion chromatograph. The sample is

pumped by the eluent stream through two (2) different

ion exchange columns: a guard column, which serves to

protect the separator column from residual particulate

matter and retain certain organics, and the separator

column, the primary function of which is to separate

analyzed ions based on their affinity for the exchange

sites of the resin. Both guard column and the separator

column are packed with identical low capacity anion

exchanger (anion analysis) or cation exchange (cation

analysis). The separated ionic species then pass to a

detector module consisting of a chemical suppressor

device and a conductivity cell. The suppressor device is

used to reduce background conductivity of the eluent to

a low, or negligible level, and convert analyte anions

into their acid form or analyte cations into their

hydroxide form. Thus, separated and modified ionic

species are detected using an electrical conductivity

cell. Anions are identified based on their retention time

compared to the known standards. Quantitation is

accomplished by measuring the peak height or area, and

comparing it to a calibration curve generated from

known standards.

NOTE 5: For recommended practice for ion chromatography

analyses, see instrument manufacturer’s literature and ASTM

D 4327.

6.5.2 Interferences

6.5.2.1 High levels of organic acids may be present in

molding compound extracts. This may interfere with

inorganic anion analysis. Two (2) common species,

formate and acetate, elute between fluoride and

chloride. This may be minimized by modifying

instrument set-up.

6.5.2.2 Certain amines may interfere with the

determination of sodium or potassium. This may be

minimized by using different instrument set-ups.