1. Central Calibration Laboratory
2. Regulator Guidelines

Standard Reference Gases

Guidelines For Standard Gas Cylinder and Pressure Regulator Use

P.M. Lang
NOAA CMDL Carbon Cycle-Greenhouse Gases
February 2, 1998

• Standard gas cylinder:

  Trace gas standards used for measuring CO2, CO, N2O, SF6, and CH4 by the Carbon Cycle-Greenhouse Gases group (CCGG) of NOAA CMDL are contained in aluminum cylinders purchased from Scott- Marrin, Riverside, California. The cylinders are treated with a proprietary passivation treatment. CCGG uses three different size cylinders but most of our standards are contained in 30 liter (internal volume) cylinders. The cylinders are ordered with brass Ceodeux cylinder valves (CGA590) containing all-metal seats and nickel stems. The cylinders are shipped to CMDL with 1380 kPa (200 psig) of dry, ultrapure air. It is important for the cylinders to be dry (and remain dry) during filling and use. Brass cylinder valves rather than stainless steel, are recommended for all trace gas species measured by CCGG.

  NOTE: Read and follow all safety procedures for handling high pressure gas cylinders.

• Pressure regulators:

  The proper regulator to use for a trace gas standard may depend on the particular trace gas being measured. The regulators CMDL uses for carbon cycle trace gas standards do not always perform well for trace gas stable isotopic measurements. Standards for SF6 measured by GC-ECD may require special high-purity electron capture sensitive regulators. CCGG uses two-stage, high purity, low flow, compact regulators on most standards. The regulators are nickel-plated brass with stainless steel diaphragms and low internal volume. The desired delivery flow rates, purity levels, and corrosiveness of the standard gas should be determined before purchasing a regulator. It is important to note that delivery pressure range and gauge delivery pressure are different. Order a regulator that is within the required delivery pressure range. (For example, a 0-700 kPa (0-100 psig) delivery pressure gauge may have a maximum delivery pressure of 350 kPa (50 psig).)

• Standard gas cylinder handling:

  After purchasing a calibrated standard gas from CCGG, the following guidelines are suggested.

  • 1. Dedicate a regulator for each standard gas cylinder. The regulator should be installed, leak checked, flushed, pressure checked, conditioned, and remain on the cylinder at all times if possible.
  • 2. Regulator installation: Follow basic cylinder/regulator installation procedures as indicated in the instructions sent with each regulator.
  • 3. Leak check: After the regulator is attached to the cylinder a leak check should be performed. The first step in this procedure differs from gas company guidelines. We allow a small amount of gas to escape the regulator when first opening the cylinder valve to prevent contamination of the standard.
    • Turn the pressure delivery handle clockwise to allow a small amount of gas to escape the regulator when the cylinder valve is opened.
    • Slowly open the cylinder valve until gas starts to escape from the regulator.
    • Close the regulator by turning the pressure delivery handle fully counterclockwise.
    • Fully open the cylinder valve.
    • Leak check the regulator/cylinder connection (CGA nut) using Snoop or another leak detector.
    • If a leak is detected, close the cylinder valve and depressurize the regulator before attempting to fix the leak.
    • After tightening the CGA nut or adjusting the position of the regulator, open the cylinder valve and recheck for leaks.
    • Once the cylinder/regulator connection is leak free we recommend an initial regulator flushing and pressure check to detect small leaks and malfunctioning regulators.
  • 4. Flushing: Both the high and low sides of a two stage regulator should be flushed (pressurized and vented) after initial installation and before each use.
    • Close the cylinder valve and turn the pressure delivery handle clockwise to allow a small amount of gas to escape the regulator outlet after the cylinder valve is opened.
    • Fully open and fully close the cylinder valve so that the low and high side gauges are pressurized and then drained to zero. (The low side pressure can be increased for faster flushing.)
    • Pressurize and vent the regulator four times.
    • Fully open the cylinder valve and turn the pressure delivery handle fully counterclockwise to close the regulator to prepare for the pressure check.
  • 5. Pressure Check: A pressure check consists of pressurizing both the low and high gauges of the regulator, letting it sit overnight, and then rechecking the pressures.
    • Plug the outlet side of the regulator at the regulator outlet, shutoff valve, or somewhere downstream of the shut off valve. Do not use the pressure delivery handle to plug the outlet.
    • Pressurize the high side by fully opening the cylinder valve.
    • Set the delivery pressure to a setting about one-half of the maximum delivery pressure by turning the pressure delivery handle clockwise.
    • Shut off the regulator by turning the pressure delivery handle fully counterclockwise.
    • Close the cylinder valve. (This is important: If there is a leak, the cylinder could be empty on the morning.)
    • Write down the initial pressure for each gauge.

    A pressure check is used to isolate different parts of the cylinder and regulator system and look for leaks. If, after closing the cylinder valve and regulator, the pressure on the high side gauge increases, then the regulator is defective and it should not be used. If the high side pressure gauge decreases, then there is a leak between the cylinder and the high side of the regulator, most likely the CGA fitting. If the high side gauge decreases and the low gauge increases, there is a leak in the regulator across the diaphragm and this regulator should not be used. If the low side gauge decreases, then there is a leak between that gauge and the downstrem shutoff.

  • 6. Conditioning: Conditioning the regulator is important to ensure that the standard air equilibrates with the regulator. After the regulator is conditioned, standard air should pass through the regulator with no gain or loss of the species of interest. The regulator should be conditioned with standard air for at least one week before use. Failure to condition the regulator may result in incorrect measurements.
    • a. After pressure checking the regulator leave it pressurized (high and low side) with the cylinder valve closed for 2 or 3 days.
    • b. Open the system downstream and flush the regulator two times using the pressurize and vent method described in #4.
    • c. Close the downstream outlet, open the cylinder valve, pressurize the regulator by turning the pressure delivery handle clockwise, then close the regulator by turning the pressure delivery fully counterclockwise, and then close the cylinder valve.
    • d. Leave the regulator pressurized for two more days.
    • e. On day 3, vent and pressurize two more times.
    • f. Repeat #6c and leave the regulator pressurized for the remainder of the week.
  • 7. Daily use: Before each use (each day) the regulator should be flushed (vented and pressurized) four times as in #4. Allow the regulator to fully depressurize before opening the cylinder valve. At the end of the day the cylinder valve should be closed, leaving the regulator pressurized (high side). The low side can also remain pressurized if there is a shut off downstream.
  • 8. Notes:
    • a. Cylinder valves can be difficult to open or close, CCGG uses gloves or some other gripping device to close hard-to-turn cylinder valves. Failure to fully close a cylinder valve may result in loss of standard air.
    • b. If a regulator is removed from the cylinder, it is important to retighten the cylinder valve after the regulator is depressurized and removed.