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SEMI C3.58-0303 © SEMI 2000, 2003 1 SEMI C3.58-0303 SPECIFICATION FOR OCTA FLUOROCYCLOBUTANE, C 4 F 8 , ELECTRONIC GRAD E IN CYLINDERS This specification was technically approved b y the Globa l Gases Com mittee and is t…

SEMI C3.39-0304 © SEMI 1989, 2004 6

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SEMI C3.58-0303 © SEMI 2000, 2003 1

SEMI C3.58-0303

SPECIFICATION FOR OCTAFLUOROCYCLOBUTANE, C

ELECTRONIC GRADE IN CYLINDERS

This specification was technically approved by the Global Gases Committee and is the direct responsibility of

the North American Gases Committee. Current edition approved by the North American Regional Standards

Committee on October 25, 2002. Initially available at www.semi.org December 2002; to be published March

0303. Originally published June 2000.

NOTICE: This entire document was completely revised in 2003.

1 Description

1.1 Octafluorocyclobutane, also known as

perfluorocyclobutane, is a gas under normal

atmospheric conditions (15°C and 760 mm Hg).

1.2 The gas is a non-flammable, non-toxic, colorless

and odorless gas which is stable under normal

conditions.

NOTICE: 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 and health practices and determine

the applicability of regulatory or other limitations prior

to use.

2 Specifications

Purity: 99.999%

Impurities Maximum Acceptable Level

Oxygen 1 ppmv

Moisture 3 ppmv

Other organic

(PFC-1216, PFC-31-10mc,

PFC-1318my, PFC-31-

10my, CFC-114, CFC-114a,

THF)

10 ppmv

Acidity (as HCl) 100 ppbw

Air (N

, O

, CO, CO

) 3 ppmv

3 Referenced Standards

None.

4 Physical Constants (for information only)

Formula C

or CF

• CF

Molecular weight 200

Melting point

−41.4°C

Boiling point

−6°C

Relative density, gas 6.9 (air = 1)

Relative density, liquid 1.6 (water = 1)

Vapor pressure 20°C

2.7 bar

Appearance/Color Colorless gas

Odor none

5 Analytical Procedures

NOTE 1: Samples of octafluorocyclobutane should be

equilibrated at no less than 30°C (85°F) for at least 24 hours

prior to analysis to ensure adequate vapor pressure for

analysis and consistency.

5.1 Acidity — This procedure is for the determination

of acidity in octafluorocyclobutane utilizing an aqueous

conductivity measurement. Calculations are made

relating sample conductivity to free acidity, calculated

as hydrochloric acid, in the sample.

5.1.1 Detection Limit — 30 ppb as HCl.

5.1.2 Apparatus: A conductivity bridge and cell, heat

gun, graduated cylinders, gas dispersion tube, wide-

mouth polyethylene bottle, hypodermic syringes,

polyethylene beaker, water purification system.

5.1.3 Reagents

5.1.3.1 Hydrochloric acid, 0.01 N standard in SDA-2B

ethyl alcohol (store the standard in separate 50-mL

serum capped vials).

5.1.3.2 CFC-11, special (analyzed to have an aqueous

conductance of < 0.5 µmho/cm). If CFC-11 is not

available, a similar degreasing solvent can be

substituted, such as HFC-43-10.

5.1.3.3 Distilled and de-ionized water, aqueous

conductivity < 0.5 µmho/cm, prepared immediately

prior to use by passing distilled water through a water

purification system and analyzing it with a conductivity

bridge. DO NOT STORE DE-IONIZED WATER FOR

USE IN THIS ANALYSIS.

5.1.3.4 RBS-35 cleaner.

5.1.4 Operating Procedure

5.1.4.1 Attach a suitable regulator to the cylinder

outlet.

SEMI C3.58-0303 © SEMI 2000, 2003 2

5.1.4.2 Conductivity bridge/cell — Store the

conductivity cell in a polyethylene beaker containing

de-ionized water when not in use.

5.1.4.3 Calibration

5.1.4.3.1 Add CFC-11 to the 20 mL calibration mark of

the polyethylene (PE) bottle. Immediately cap the

bottle and shake contents vigorously for approximately

30 seconds. Discard the CFC-11.

5.1.4.3.2 Fill the bottle again with CFC-11 to the 20

mL mark. Immediately add 100 mL of de-ionized (DI)

water to the bottle, cap and shake vigorously for

approximately 120 seconds.

5.1.4.3.3 Rinse the conductivity cell with DI water and

shake it dry. Uncap the PE bottle and dip the

conductivity cell into the water layer (top layer). Read

and record the conductivity value. This reading will

serve as the “BLANK” value. Remove the conductivity

cell from the solution, rinse with DI water and store in a

beaker containing DI water. Immediately cap the PE

bottle.

5.1.4.3.4 Fill and flush a clean, dry, 50 microliter

syringe several times with the 0.01 N standard,

hydrochloric acid in SDA-2B ethanol. Fill the syringe

to a volume of 30 microliters. Holding the syringe

vertically with needle pointing up, tap the barrel gently

to permit air bubbles to rise to the top. Slowly depress

the plunger until the plunger tip is aligned exactly with

the 20 microliter mark. Immediately uncap the PE

bottle and inject the syringe contents into the bottle.

Immediately cap the bottle. Shake the bottle vigorously

for approximately 120 seconds. Uncap the PE bottle

and dip the conductivity cell into the water layer. Read

and record the conductivity value. Remove the

conductivity cell from the solution, rinse with DI water

and store in a beaker containing DI water.

5.1.4.3.5 Calculate the nanograms (ng) of hydrochloric

acid used in the standard from the following equation:

ng HCl = V × N × MEQ × 10

Where: ng HCl = nanograms of HCl in

the standard

V = HCl volume, microliters

N = HCl normality

MEQ = HCl milliequivalent weight

(g/meq) = 0.036461

5.1.4.3.6 Calculate the calibration factor as follows:

ng HCl/µmho = A

(C2-C1)

Where: ng HCl/µmho = calibration

factor

A = ng HCl in standard

C1 = blank conductivity, µmho

C2 = standard conductivity, µmho

5.1.4.3.7 Repeat procedure at least six times. Use the

average of the six calibration factors for sample

calculations.

5.1.4.4 Samplying and Analysis

5.1.4.4.1 Add CFC-11 or a similar degreasing solvent

to the 20 mL calibration mark of the polyethylene (PE)

bottle. Immediately cap the bottle and shake contents

vigorously for approximately 30 seconds. Discard the

CFC-11.

5.1.4.4.2 Fill the bottle again with CFC-11 to the 20

mL mark. Immediately add 100 mL of DI water to the

bottle, cap and shake vigorously for approximately 120

seconds.

5.1.4.4.3 Rinse the conductivity cell with DI water and

shake it dry. Uncap the PE bottle and dip the

conductivity cell into the water layer (top layer). Read

and record the conductivity value. This reading will

serve as the “BLANK” value. Remove the conductivity

cell from the solution, rinse with DI water and store in a

beaker containing DI water. Immediately cap the PE

bottle.

5.1.4.5 Weigh the sample cylinder and record. Attach

PE gas dispersion tube to the sample cylinder valve.

Uncap the PE bottle and lower the gas dispersion tube

into the water. Open the cylinder valve and purge

sample through the bottle such that about 150 g of

sample are added to the bottle over a 60 minute period.

Close the cylinder valve and immediately remove the

gas dispersion tube and cap the bottle. Record the final

weight of the capped sample cylinder.

5.1.4.6 Shake the PE bottle vigorously for

approximately 120 seconds. Read and record the

conductivity value as done previously.