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SEMI G29-1296 E © SEMI 1986, 2002 3 6.5.3 Apparat us 6.5.3.1 Ion ch romatograph (Dionex or equivalent). The chromatograph shall be equip ped with an injection valve, a 50–100 µ l sample loop, and shall be set up with the…

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.

SEMI G29-1296

6.5.3 Apparatus

6.5.3.1 Ion chromatograph (Dionex or equivalent). The

chromatograph shall be equipped with an injection

valve, a 50–100 µ l sample loop, and shall be set up with

the following:

1. Guard Column

2. Separator Column

3. Chemical Suppressor Device

4. Conductivity Detector

6.5.4 Reagents

6.5.4.1 Water Purity — Water used in the preparation

of eluents, standards, and sample extraction shall

conform to ASTM D 1193.

6.5.4.2 Reagent Purity — Reagent grade chemicals

should be used in all tests.

6.5.4.3 Eluent/Regenerant Solutions — Should be

prepared in accordance with instrument manufacturer’s

instructions recommended for each column set.

6.5.4.4 Stock Solutions — Stock solutions (1 ml - 1 mg

- 1 ppm ion of interest) should be prepared according to

accepted practice, and as described in the instrument

manufacturer’s instructions.

6.5.4.5 Calibration Standards — Prepare a blank and

at least three (3) different calibration solutions

containing combination of anion/cations. These

solutions must be prepared in volumeric flasks (see

Table 1).

6.5.4.5.1 Prepare a standard solution I by diluting the

volume of each anion/cation stock solution as specified

in Table 1 together with 1 litre of water.

6.5.4.5.2 Prepare a standard solution II by diluting 20

ml of standard solution II to 100 ml with water (see

Table 1).

NOTE 6: If the concentrations of the sample ions are known,

or estimated, the concentration of calibration standard

solutions may be varied to better approximate or bracket

concentration range of interest.

6.5.5 Calibration

6.5.5.1 Analyze the blank and each of the prepared

calibration solutions described in Section 6.5.4.5.

6.5.5.2 Prepare analytical curves for each anion/cation

of interest by plotting on linear graph paper peak height

or peak area versus nominal concentrations of the

anion/cation calibration standard.

NOTE 7: Each analytical curve should be established using

only one (1) scale setting.

6.5.6 Procedure

6.5.6.1 Set-up the ion chromatograph according to the

manufacturer’s instructions.

NOTE 8: The range setting required for the analysis will

depend on the concentration of ions in the sample and should

be chosen accordingly. For these types of samples, operating

range from 30 to 30µ S/cm, full scale is most frqurntly used.

6.5.6.2 Equilibriate the system by pumping eluent

through the analytical system until a stable baseline is

obtained (approximately twenty (20) minutes).

6.5.6.3 Filter samples through a pre-washed 0.22 µ m

filter prior to analysis.

NOTE 9: Several types of syringe-tip filters are available

(Millipore or equivalent).

6.5.6.4 Load 2–3 ml of sample into the injection part

using a syringe. Inject the sample into the eluent stream

and record the ion chromatogram.

6.5.7 Calculations

6.5.7.1 Refer to the peak height or area for the

anions/cations of interest to the appropriate analytical

curves to determine the anion concentration.

6.6 Inductivity Coupled Argon Plasma

Spectrometry/ICP

6.6.1 Method Principle — Inductivity coupled Argon

Plasma (ICP) uses high frequency Argon Plasma to

excite sample constituents to 8000° K. Because the

plasma ionizes most atomic species, background

interferences are vastly reduced and linear response

over several orders of magnitude can be observed for

most elements. The sample extract is aspirated into the

plasma by means of a high purity argon carrier gas. The

resulting emissions are directed into the spectrometer

and signal strengths are read by photomultiplier tubes

placed at emission points in a focal curve. A computer

is used to scan each elemental channel many times a

second, and this output is sent to a printer in numerical

form. The cycle or time of analysis is usually about

seven (7) seconds. With this instrument, very little of

the extracted sample is consumed.

SEMI G26-1296

6.6.2 Instrument Conditions

Typical operating conditions are:

Excitation source 27 MHz plasma

Carrier gas 99.999% Argon

Sample flow 1 ml/min

Power output 1000 watts

Plasma temperature 8000° K

Slit width of Spectrometer 30 µ m

6.6.3 Measurement of Sodium, Potassium, and Antimony — A standard solution of ten (10) ppm of sodium,

potassium, and antimony should be prepared and cycled through the ICP instrument. The blank extract sample and

the unknown molding compound extracts are then run through the ICP. The values obtained for sample are corrected

by subtracting values obtained for the blank. With the ICP, sodium, potassium, and antimony can be analyzed with

sensitivities to the ten (10) PPB levels. Any additional elements present may be obtained on the same cycle with no

additional preparation.

Table 1 Preparation of Standard Solutions for Instrument Calibration

Standard Solution

Anion

ml of Stock Soln. Diluted

to 1000 ml

Anion Conc. mg/1

Standard Solution II

Standard Solution III

Chloride (Cl) 5 5 1 0.2

Phosphate (HPO

) 25 25 5 1.0

Bromide (Br

) 10 10 2 0.4

Nitrate (NO

30 30 6 1.2

Sulfate (SO

) 25 25 5 1.0

Cation

Sodium (NA

) 5 5 1 0.2

Ammonium (NH

) 5 5 1 0.2

Potassium (K

) 10 10 2 0.4

NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for

any particular application. The determination of the suitability of the standard is solely the responsibility of the user.

Users are cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant

literature respecting any materials mentioned herein. These standards are subject to change without notice.

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