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SEMI C3.34-1102 © SEMI 1989, 1102 3 8.3.2 Instrum ent Param eters 8.3.2.1 Columns: Column 1: Porapak QS 2.5 m (8 ft) by 3.2 mm (1/8 in) OD ss or equivalent. Column 2: 5A Molecular sieve, 3 m (10 ft) by 3.2 mm OD ss or eq…

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SEMI C3.34-1102 © SEMI 1989, 2002 2
chromatograph with a methanizer and a flame
ionization detector. (See Figure 1, Notes 3 and 4.)
NOTE 3: An optional temperature ramping during vent will
shorten the analysis time.
NOTE 4: Carrier gases should contain less than 0.1 ppm
carbon monoxide and less than 0.1 ppm carbon dioxide.
8.1.1 Detection Limit — 0.1 ppm for each impurity.
8.1.2 Instrument Parameters
8.1.2.1 Column: Porapak QS 3 m (10 ft) by 1.6 mm
(1/16 in) ID ss or equivalent.
8.1.2.2 Carrier Flow: 30 mL/min helium.
8.1.2.3 Sample Volume: 1.5 mL.
8.1.2.4 Support Gases: As specified by the instrument
manufacturer.
Hydrogen: 20–30 mL per min added to the carrier gas
between the column outlet and the methanizer inlet.
Air: 500 mL/min.
8.1.2.5 Temperatures:
Detector 110°C
Injector 60°C
Oven 60°C
Methanizer 370°–400°C
8.1.3 Calibration Standards — 1–10 ppm carbon
monoxide, 1–10 ppm carbon dioxide, balance helium.
8.1.4 Operating Procedure
8.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. The order of elution is carbon
monoxide, carbon dioxide. Repeat this operation.
8.1.4.2 Inject the sample to be tested in same manner
as the calibration standard and vent after elution of
carbon dioxide is completed, in case any silane is
present. Record the retention times and peak areas.
8.1.4.3 Repeat Section 8.1.4.1.
8.1.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of carbon monoxide
and carbon dioxide using the formula below. The
results may not exceed the specifications in Section 7 of
this standard.
Sample of
ionConcentrat
Standard of
ionConcentrat
AreaPeak Standard
AreaPeak Sample
=×
8.2 Methane, Ethane, Propane, and Silane — This
procedure is for the determination of hydrocarbons
(methane, ethane, and propane) and silane in disilane
using a gas chromatograph with a thermal conductivity
detector.
8.2.1 Detection Limit — 3 ppm for each impurity.
8.2.2 Instrument Parameters
8.2.2.1 Column: Porapak QS 3 m (10 ft) by 1.6 mm
(1/16 in) ID ss or equivalent.
8.2.2.2 Carrier Flow: 25 mL/min helium.
8.2.2.3 Sample Volume: 1 mL.
8.2.2.4 Temperatures:
Detector 80°C
Injector 60°C
Oven 60°C
8.2.3 Calibration Standards — 10–50 ppm methane,
5–10 ppm ethane, 5–10 ppm propane, 0.1–1% silane,
balance helium.
8.2.4 Operating Procedure
8.2.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. Order of elution is methane, silane,
ethane, propane.
8.2.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention times
and peak areas.
8.2.4.3 Repeat Section 8.2.4.1.
8.2.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of methane, silane,
ethane, and propane, using the formula below. The
results may not exceed the specification in Section 7 of
this standard.
Sample Peak Area
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample
8.3 Hydrogen, Nitrogen, and Argon — This procedure
is for the determination hydrogen, nitrogen, and argon
in disilane using a gas chromatograph with a helium
ionization detector.
8.3.1 Detection Limit — 100 ppb for hydrogen and
argon, 500 ppb for nitrogen.
SEMI C3.34-1102 © SEMI 1989, 1102 3
8.3.2 Instrument Parameters
8.3.2.1 Columns:
Column 1: Porapak QS 2.5 m (8 ft) by 3.2 mm (1/8
in) OD ss or equivalent.
Column 2: 5A Molecular sieve, 3 m (10 ft) by 3.2
mm OD ss or equivalent.
8.3.2.2 Carrier Flow: 25 mL/min helium.
8.3.2.3 Sample Volume: 3 mL.
8.3.2.4 Temperatures:
Detector 100°C
Injector 30°C
Oven 30°C
8.3.3 Calibration Standards — 1–10 ppm nitrogen, 1–
10 ppm argon, 10–100 ppm hydrogen, balance helium.
8.3.4 Operating Procedure
8.3.4.1 Determination of the backflush time: Inject a
methane sample (1–1000 ppm, balance helium) using a
10 port gas valve and backflush at different times.
Select the backflush time so that the methane peak is
split by the backflush.
8.3.4.2 Inject the calibration standard into the column
using a gas sampling valve. Backflush at the time
determined in Section 8.3.4.1. Record retention times
and peak areas. Order of elution is hydrogen, argon,
nitrogen.
8.3.4.3 Inject the sample to be tested in same manner
as the calibration standard. Backflush at the time
determined in Section 8.3.4.1. Record the retention
times and peak areas.
8.3.4.4 Repeat Section 8.3.4.2.
8.3.4.5 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of hydrogen,
nitrogen and argon using the formula below. The results
may not exceed the specifications in Section 7 of this
standard.
Sample Peak Area
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample
8.4 Disiloxane, Monoethylsilane, Trisilane, and
Tetrasilanes — This procedure is for the determination
of disiloxane, monoethylsilane, trisilane, and
tetrasilanes in disilane using a gas chromatograph with
a thermal conductivity detector.
8.4.1 Detection Limits — 5 ppm for disiloxane and 10
ppm for each of the other impurities.
8.4.2 Instrument Parameters
8.4.2.1 Column: 30% DC 200 on Chromosorb P,
80/100 mesh, 10 m (33 ft) by 3.2 mm (1/8 in) ss or
equivalent.
8.4.2.2 Carrier Flow: 20 mL/min helium.
8.4.2.3 Sample Volume: 1 mL.
8.4.2.4 Temperatures:
Detector 120°C
Injector 60°C
Oven 60°C for 25 min then 10°C/min to 120°C
8.4.3 Calibration Standard — 100 ppm each of
trisilane, i-tetrasilane, and n-tetrasilane, and 10 ppm
each disiloxane and monoethylsilane in helium. If one
or several components cannot be obtained, use a 100
ppm monosilane standard and apply the following
correction factors using the formula below (See
Reference 1).
Trisilane CF = 0.54
i-tetrasilane CF = 0.42
n-tetrasilane CF = 0.41
Correction factors for disiloxane and monoethylsilane
are not available. Use the same as disilane CF = 0.69.
concentration of impurity = calculated concentration,
using silane standard, × CF.
8.4.4 Operating Procedure
8.4.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record retention times and
peak areas. Order of elution is disiloxane, disilane,
monoethylsilane, trisilane, i-tetrasilane, and n-
tetrasilane.
8.4.4.2 Inject the sample to be tested in same manner
as calibration standard. Record the retention times and
peak areas.
8.4.4.3 Repeat Section 8.4.4.1.
8.4.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of disiloxane,
disilane, monoethylsilane, trisilane, i-tetrasilane, and n-
tetrasilane, using the formula below. If necessary,
correct the results using the specified correction factors
in Section 8.4.3. The results may not exceed the
specifications in Section 7 of this standard.
SEMI C3.34-1102 © SEMI 1989, 2002 4
Sample Peak Area
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample
8.5 Water — This procedure is for the determination of
moisture in disilane using a continuous flow
electrolysis of water in a phosphorus pentoxide (P
2
O
5
)
cell.
NOTE 5: Direct gases for moisture measurement to the
analyzer with stainless steel lines which have been purged.
8.5.1 Detection Limit — 1 ppmv
8.5.2 Flow Requirement — Set the sample flow rate
and pressure in accordance with manufacturer's
instructions.
8.5.3 Operating Procedure
8.5.3.1 Direct samples of three standards,
independently verified with a dewpoint/frostpoint
hygrometer, spanning the range of moisture content of
interest to the analyzer. After a stable reading is
obtained, record the instrument's response to each
standard.
8.5.3.2 Obtain a representative sample of the gas to be
analyzed and direct it to the unit as with the standards.
After a stable reading is obtained, record the
instrument’s response.
8.5.3.3 Construct calibration curve from the standard
data and determine the moisture content in sample gas.
The result may not exceed the specification in Section 7
of this standard.
8.6 Total Chlorides — This procedure is for the
determination of total hydrolyzable chlorides in disilane
by titration of a hydrolyzed sample of disilane. (See
Figure 2.)
8.6.1 Detection Limit — 0.5 ppm.
8.6.2 Instrument Parameters
8.6.2.1 Equipment
1. Safety purge regulator with proper fittings.
2. Flow meter capable of measuring 0.25 standard
liters per minute (0.5 SCF/hour) (Brooks or
equivalent).
3. One cylinder of nitrogen with regulator.
4. One ice bath.
5. Three magnetic stirring bars.
6. Two 2000 mL heavy-duty sidearm flasks (Fisher
Cat. No. 10-181G or equivalent).
7. One #9 one-hole rubber stopper.
8. One #9 two-hole rubber stopper.
9. Two borosilicate glass tubes with fritted cylinders
(Fisher Cat. No. 11.138B or equivalent).
10. One gas washing bottle with fritted cylinder, 125
mL cap. (Fisher Cat. No. 03-040A or equivalent).
11. One buret, 50 mL capacity with PTFE stopcock
(Fisher Cat. No. 03-700-22C or equivalent).
12. One buret stand (Fisher Cat. No. 14-688 or
equivalent).
13. Miscellaneous clamps, support stands, and rubber
hose.
14. Two 250 mL Erlenmeyer flasks.
8.6.3 Reagents
1. Potassium hydroxide flakes, technical (Fisher Cat.
No. P-246 or equivalent).
2. Mercuric nitrate crystal (Fisher Cat. No. M-168 or
equivalent).
3. Sodium chloride crystal (Fisher Cat. No. S-271 or
equivalent).
4. Diphenyl carbazone (Fisher Cat. No. D-86 or
equivalent).
5. Bromophenol blue (Fisher Cat. No. B-392 or
equivalent).
6. Nitric acid (Fisher Cat. No. AA-200 or equivalent).
7. Ethanol, denatured (Fisher Cat. No. AA-407 or
equivalent).
8.6.4 Operating Procedure
8.6.4.1 Fill each 2000 mL sidearm flask with about
1700 mL of 15% potassium hydroxide solution (15 g
KOH per each 100 mL water).
8.6.4.2 Fill the gas washing bottle with about 75 mL of
deionized water that has been degassed.
8.6.4.3 Assemble apparatus as shown in Diagram A
and purge entire system with nitrogen for 30 minutes.
8.6.4.4 Pass 30 liters (approximately one cubic foot) of
disilane through the system at a rate of 0.25 liters per
minute. Record the volume of the disilane sample.
8.6.4.5 Stop disilane flow and purge system for 30
minutes.
8.6.4.6 Remove gas washing bottle from system and
transfer contents quantitatively and with the aid of three
25 mL deionized water washings, to a 250 mL
Erlenmeyer flask.
8.6.4.7 Add a few drops of indicator solution (5 g
diphenyl carbazone plus 0.5 g bromophenol blue
dissolved in 750 mL ethanol, plus 250 mL deionized
water).
8.6.4.8 Add, in a drop-wise fashion, sufficient 0.2N
HNO
3
(13 mL conc. HNO
3
, diluted to 1 L in deionized
water) in order to just turn the solution to yellow from
purple.