GB/T 15909-2017Gas for electronic industry - Silane (English PDF)

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4.5 Determination of water content Follow

GB/T 5832.1. Before introducing the silane product, dry nitrogen can be used to completely blow out the air in the instrument system. It is permitted to use other equivalent methods to determine the moisture content in silane gas for electronic industry. Where there is a dispute over the determination results, the method specified in

GB/T 5832.1 shall be used as the arbitration method. Detection limit: 0.05×10-6 (volume fraction).

4.6 Determination of the content of metals and other elements

4.6.1 Instruments Use inductively coupled plasma mass spectrometry (ICPMS) to determine the content of metals such as aluminum, antimony, arsenic, boron, gallium, phosphorus, chromium, copper, iron, nickel, zinc and other elements in silane. Detection limit: no more than 0.01 µg/L.

4.6.2 Materials and reagents

4.6.2.1 Nitric acid: The content of metals and other elements is less than 0.01 µg/L.

4.6.2.2 Determination absorption solution: 5% nitric acid.

4.6.2.3 Standard solutions of metals and other element ions: The content of metals and other elements in the standard solution shall be close to the corresponding content in the test sample.

4.6.2.4 Alkali absorption solution: 10% ~ 20% sodium hydroxide aqueous solution.

4.6.2.5 Test water: in accordance with the requirements of Grade EW-I in GB/T 11446.1.

4.6.2.6 Polytetrafluoroethylene gas-washing bottle: 50 mL.

4.6.2.7 Conical flask for alkali solution absorption: 2 000 mL, containing 1 500 mL of alkali absorption solution.

4.6.2.8 Pipette.

4.6.2.9 Rotor flow meter.

4.6.3 Sample absorption

4.6.3.1 See Appendix A for the absorption device diagram.

4.6.3.2 Before sampling, use high-purity nitrogen to fully purge the gas line and valves.

4.6.3.3 After purging, use a pipette to accurately transfer 30 mL of absorption solution into the gas-washing bottle; after using nitrogen to purge for about 30 minutes, turn off the nitrogen, slowly open the silane cylinder, and adjust the flow rate; introduce about 20 L of silane at a flow rate of 300 mL/min; record the amount of absorbed silane sample. Record the values of atmospheric pressure and temperature.

4.6.3.4 After absorption is completed, use nitrogen to purge the gas line for about 30 minutes; turn off the nitrogen and remove the gas-washing bottle.

4.6.3.5 Make a nitrogen blank simultaneously.

4.6.4 Determination steps

4.6.4.1 Starting the instrument Turn on the instrument according to the inductively coupled plasma mass spectrometer (ICPMS) manual; adjust the various components of the instrument to meet the measurement conditions; start the measurement after the instrument is stable.

4.6.4.2 Determination 4.6.4.2.1 Determination of standard samples Inject the standard solution of metals and other elements. Record the signal intensity of metals and other elements in the standard solution. Repeat the injection of each standard solution at least twice until the relative deviation of the two parallel measurements is no more than 5%; take the average value. 4.6.4.2.2 Determination of samples Inject the sample solution after absorption under the same measurement conditions as the standard solution; record the signal intensities of different metals and other elements; repeat the injection at least twice until the relative deviation of the two parallel measurements is no more than 15%; take the average value. 4.6.4.2.3 Determination of blank Determine the blank absorption solution in the same manner as the sample.

4.6.5 Calculation of sample volume Calculate the sample volume according to Formula (3): - production date or batch number, filling mass (kg); - a reference to this Standard, technical indicators and inspector number.

5.1.12 Silane products shall be stored in a cool, dry, ventilated warehouse, away from exposure to sunlight and away from heat sources.

5.2 Safety warning

5.2.1 Silane is a colorless, flammable gas with a special odor at room temperature and pressure. It will produce a violent chemical reaction when in contact with fluorine, chlorine, etc.

5.2.2 When the mixed gas leaks into the air, the lower ignition limit of silane is about 0.8×10-2 (volume fraction).

5.2.3 When extinguishing a fire, firefighters shall wear gas masks and full-body fire suits and extinguish the fire in the upwind direction. Cut off the gas source; move the container away from the fire scene to an open area as much as possible; spray water to keep the container cool until the fire is extinguished; and use water mist to reduce the formation of combustion products in the air. Do not spray water directly onto the burning silane. If the gas source cannot be cut off, do not extinguish the flame at the leak. Fire extinguishing agents: water, foam, dry powder, carbon dioxide. Freon fire extinguishers shall not be used.

5.2.4 In case of leakage, quickly evacuate personnel from the leakage contaminated area to the upwind area, isolate it, and strictly restrict entry and exit. Cut off the fire source. It is recommended that emergency personnel wear self-contained positive pressure respirators and anti-static work clothes. Enter the scene from the upwind area. Cut off the leakage source as much as possible. Dilute with spray water. If possible, send the residual gas or leaked gas to the water washing tower or the fume hood connected to the tower with an exhaust fan. Leaking containers shall be properly handled and used after repair and inspection.

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