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SEMI C3.34-1102 © SEMI 1989, 1102 5 8.6.4.9 Titrate wi th a solution of 5 g. m ercuric nitrate Hg(NO 3 ) 2, (diluted to 1000 mL in de ionized water; then 50 mL diluted t o 500 mL in d eionized water ) which has been prev…

SEMI C3.34-1102 © SEMI 1989, 2002 4

Sample Peak Area

Standard Peak Area

oncentrat

of Standard

oncentrat

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

)

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

(13 mL conc. HNO

, diluted to 1 L in deionized

water) in order to just turn the solution to yellow from

purple.

SEMI C3.34-1102 © SEMI 1989, 1102 5

8.6.4.9 Titrate with a solution of 5 g. mercuric nitrate

Hg(NO

)

(diluted to 1000 mL in deionized water; then

50 mL diluted to 500 mL in deionized water) which has

been previously standardized to 5.0 mL of a sodium

chloride solution (approximately 165 ng NaCl,

accurately weighed, dissolved in 100 mL deionized

water).

8.6.5 Calibration

8.6.5.1 Run titration blank consisting of 150 mL

deionized water.

8.6.5.2 Calculate the concentration of chloride, using

the formula below. The result may not exceed the

specification in Section 8 of this standard.

mL sample - mL blank

mL standard - mL blank

wt. of NaCl g

()

100.0 mL

60.66% Cl

100% NaCl

1000 mL

1 L

.005 L

35.453 g/mole

0.082 atm L/mole

1 atm

294.26

volume of gas samples

ppm = ppm Cl

8.6.6 Final Calculation — Convert the results from

ppm to ppm-wt using the formula below. The result

may not exceed the specification in Section 7 of this

standard.

ppm- wt = ppm mole/mole()×

35.45

62.22

FIP

Figure 1

G.C. Configuration

Figure 2

Chloride Scrubbing Apparatus

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