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SEMI C3.58-0303 © SEMI 2000, 2003 4 6.3.3 Operation Check — The instrument sho uld be checked p eriodically for correct operation. The instr ument should be zero ed by flowing refere nce gas, whic h is dry oc tafluorocyc…

SEMI C3.58-0303 © SEMI 2000, 2003 3

5.1.4.6.1 Calculate the sample’s free acidity using the

following equation:

ppb HCl = (C2-C1) × F

Where: ppb HCl = free acidity

C1 = blank conductivity, µmho/cm

C2 = sample conductivity, µmho/cm

F = calibration factor, ng HCl/µmho

W = sample weight used in analysis,

grams

6 Analytical Procedures - Instrumental

Analysis

6.1 Air (N

, CO, CO

) and Oxygen — This

procedure is for the determination of air components in

octafluorocyclobutane using a gas chromatograph with

a discharge ionization detector. Column switching is

used to separate and elute the components and to

backflush octafluorocyclobutane. One method/column

is used for N

, O

, and CO and a second

method/column is used for CO

. The sample should be

taken from the vapor in the container directly into the

instrument sampling system. The container being

analyzed should have equilibrated at approximately

30°C before analysis is begun.

6.1.1 Detection Limits — Nitrogen, 10 ppb vol;

Oxygen, 50 ppb vol; Carbon monoxide, 10 ppb vol;

Carbon dioxide, 10 ppb vol.

6.1.2 Instrument Parameters

6.1.2.1 Columns: Precolumn: Haysep DB on

Carbopack B, 80/100 mesh, 2 ft × 1/8 in stainless steel.

, O

, CO column: Molecular Sieve 5a, 80/100 mesh,

8 ft × 1/8 in stainless steel. CO

column: Haysep DB

on Carbopack B, 80/100 mesh, 8 ft × 1/8 in stainless

steel.

6.1.2.2 Gas Flows: Helium carrier gas 40 mL/min for

each column.

6.1.2.3 Sample volume: 1.0 mL

6.1.2.4 Temperatures: Detector setpoint = 25°C

(actual is higher ~60°C due to proximity to the oven),

Oven 77°C isothermal.

6.1.2.5 Calibration Standard: 1-30 ppm vol oxygen,

nitrogen, carbon monoxide, and carbon dioxide in

helium.

6.1.2.6 Chromatograms — See Figures 1,2.

6.2 Organic Impurities — This procedure is for the

determination of organic impurities in

octafluorocyclobutane using a gas chromatograph with

a packed column and flame ionization detector.

6.2.1 Detection Limits

PFC-1216 (hexafluoropropene),

PFC-31-10mc (n-decafluorobutane),

PFC-1318my (octafluorobutene, cis and trans)

0.1 vol, ppm

PFC-31-10my (iso-decafluorobutane),

CFC-114 (1,2-dichloro-1,1,2,2-tetrafluoroethane),

CFC-114a(1,1-dichloro-1,2,2,2-tetrafluoroethane),

THF(tetrahydrofuran)

0.2 vol, ppm

6.2.2 Instrument Parameters

6.2.2.1 Column — 1% SP-1000, on Carbopack B,

60/80 mesh, 24 ft × 1/8 in stainless steel or equivalent.

6.2.2.2 Gas Flows — Helium carrier gas, 20

mL/minute.

6.2.2.3 Sample volume — 1.0 mL vapor.

6.2.2.4 Temperatures — Injector = 150°C, Detector =

250°C, Oven: 75°C for 10 minute, increase 8°C/min to

200°C and hold for 10 minutes.

6.2.2.5 Calibration Standard: 1-50 ppm vol, PFC-

1216, PFC-31-10my, PFC-31-10mc, PFC-1318my (cis

and trans), CFC-114/114a, and THF in

octafluorocyclobutane.

6.2.2.6 Chromatogram — See Figure 3.

6.3 Water — This procedure is for the determination of

trace moisture (water) in Octafluorocyclobutane, using

oscillating crystal technology. The instrument monitors

the change in vibrational frequency of a

hygroscopically sensitized quartz crystal when it is

exposed alternately to wet and dry sample gas. The

change in vibrational frequency is a function of the

amount of moisture sorbed from the wet sample gas.

The sample should be taken from the vapor in the

container directly into the instrument sampling system.

The container being analyzed should have equilibrated

at approximately 30°C before analysis is begun.

6.3.1 Detection Limit — 0.04 ppm vol (40 ppb vol).

6.3.2 Sample Pressure and Flow — These parameters

should be set in accordance with instrument

manufacturer’s instructions.

6.3.3 Operation Check — The instrument should be checked periodically for correct operation. The instrument

should be zeroed by flowing reference gas, which is dry octafluorocyclobutane (dried by use of an ultra dryer system

provided by the instrument manufacturer). Then the instrument should be calibrated by use of the internal moisture

generator (permeation tube) which has been certified by the manufacturer at some known moisture level. When not

in use the instrument should be purged with dry gas (i.e., helium or nitrogen).

6.3.4 Operation Procedures

6.3.4.1 Initiate flow of the reference gas to the instrument and allow 30 minutes for stabilization.

Figure 1

Nitrogen, Oxygen, and Carbon Monoxide Determination in Octafluorocyclobutane

Figure 2

Carbon Dioxide Determination in Octafluorocyclobutane

Figure 3

Determination of Organic Impurities in Octafluorocyclobutane

6.3.4.2 Obtain a continuous flow sample of the Octafluorocyclobutane source. The sample system by which the

octafluorocyclobutane is passed to the instrument should consist of electroplated stainless steel tubing, zero dead-

volume fittings, and be heated and purged with dry gas while not in use.

6.3.4.3 Allow the sample gas to flow through the sampling system and instrument until a stable reading is obtained.

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