Applicable regulations and safety rules for supercritical CO2

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Regulatory manufacturing constraints

In compliance with the regulatory texts cited, the solution is CE marked and delivered with a CE certificate of conformity, verified with the "anomaly detection grid" of INRS ED 4450.
The noise level is less than 80 dB in operation.
The CO2 installation and its storage are not classified ICPE.
Our CO2 machines comply with the following 5 directives:

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Regulations governing machine operation

As for machine operation, it is governed by Ministerial Order TREP 1723392A of 20/11/2017 on the in-service monitoring of pressure equipment and simple pressure vessels.
Two steps are particularly important to observe:

  • Periodic inspection :
    The periodic inspection of pressurized volumes is the responsibility of the operator. It must be carried out by a notified body duly appointed by the operator.
    Dense Fluid Degreasing will provide assistance to the operator for the organization and preparation of the periodic inspection.

    OR Every 24 months for each pressure equipment: of category "ACAFR" or "Autoclave à Couvercle Amovable à Fermeture Rapide" meeting the criterion "greater than or equal to 10.

    OR Every 48 months for all non-"ACAFR" pressure equipment not meeting the "greater than or equal to 10,000 Bar x liter" criterion, considering commissioning as an operator.

    It should be noted that this Periodic Inspection involves a temporary production stop.
  • Periodic requalification :
    A periodic requalification of pressurized volumes is carried out every 10 years from the time the equipment is "commissioned".
    The requalification is the responsibility of the operator, and must be carried out by a notified body duly appointed by the operator. Support provided by our maintenance teams includes:
    - Preparation of equipment
    - Filling with water
    - Pressure testing (hydraulic test), in the presence of the notified body appointed by the operator
    - Draining, drying
    - Replacement of safety valves
    - Checking of safety systems
    - Reassembly

    Dates of intervention defined by mutual agreement so as not to disrupt production, as this implies a production stop, depending on the length of stop required.

Safety, environment and supercritical CO2

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Emission Limit Values

The CO2 used is not produced by the machine. Therefore, it is not subject to any emission standards. There are no specific emission limits for supercritical CO2 itself, as it is a natural gas present in the atmosphere.

However, when supercritical CO2 is used as a solvent in industry, it is important to ensure that CO2 emissions are controlled to minimize environmental impacts. It is important to ensure that the CO2 used is recovered and reused to avoid unnecessary leaks and emissions.

To minimize carbon dioxide emissions to the absolute minimum, our new equipment can be equipped with a recovery system that achieves a recovery rate exceeding 99%.

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Exposure Limit Values

Our cleaning or supercritical CO2 extraction machines adhere to the Occupational Exposure Limit (OEL) for CO2 of 5000 ppm under normal working conditions of 8 hours per day. All our installations come equipped with the necessary CO2 sensors to detect and alert to any potential CO2 presence risk.

The machine's body incorporates its ventilation system for capturing carbon dioxide, even in the event of a leak.

Your questions ?

Our answers !

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Where does the CO2 used in our machines come from?
Our machines do not produce CO2; they solely use CO2 sourced from external storage. The carbon dioxide used is, in fact, a byproduct generated during various industrial processes, including the chemical industry and methane production. This CO2 is then captured, purified, and reprocessed by gas companies such as Air Liquide, Messer, Linde Gas, etc. Air Liquide has been the historical gas partner of Dense Fluid Degreasing, but gas companies now use standardized fittings for their bottles, spheres, or external tanks due to regulatory standards. Therefore, our CO2 equipment can adapt to all gas companies. There are three grades of CO2 that can be used in our machines.
  • The food-grade CO2 is the most widespread and commonly used grade of CO2. It is the same grade of CO2 used in the food industry to carbonate beverages like sodas, some beers, sparkling water, etc. This gas is 99.9% pure, with the remaining 0.1% consisting of various impurities, including oxygen and sulfur.
    For example, at Air Liquide, this food-grade CO2 is sold under the name "ALIGAL."
  • The medical-grade CO2 is a grade of CO2 used particularly in medical, research, or analytical applications. It is 99.998% pure, with the remaining 0.002% consisting of various impurities, including oxygen and sulfur.
    At Air Liquide, this medical-grade CO2 is marketed under the name "ALPHAGAZ."
  • The pharmaceutical-grade CO2, primarily used in the pharmaceutical sector and recommended for specific industries like aerospace or space, is 99.5% pure. Similar to the previous grades, the remaining 0.5% consists of impurities. However, these impurities are different from the first two grades, which is why this grade is favored by specific industries.
    At Air Liquide, this pharmaceutical-grade CO2 is referred to as "PHARGALIS."
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What are the types of CO2 storage?
When CO2 is stored, it is typically kept in its liquid state. It is commonly maintained at 20°C and 60 bars of pressure to remain in this state. It can be stored in three different types of packaging:
  • In bottles, ranging from XL to XL sizes, they have the advantage of being easy to store and transport. They must be placed in a metal frame to keep them upright. Bottle storage is suitable for moderate usage of Dense Fluid Degreasing machines, such as a few days per week or for small autoclave volumes. Bottles are also preferred for applications requiring pharmaceutical or medical-grade CO2 due to the cost associated with these specific grades.
    This packaging method is allowed indoors.
  • In 300kg CO2 spheres, like bottles, they are easy to move and also placed in a metal frame to keep them upright. The use of spheres is recommended for annual consumption of up to 7 tonnes per year.
    This packaging method is allowed indoors.
  • In tanks or external storage. The smallest tanks have a minimum capacity of 3.5 tonnes. Automatically replenished by the gas company, which can remotely monitor the remaining CO2 level and, based on regular consumption, schedule a delivery without prior request. Using a tank requires the installation of a CO2 transport system from the tank to the Dense Fluid Degreasing machine. This operation is carried out in coordination with the chosen gas company.
    This packaging method is primarily installed outdoors.

Regarding the cost of CO2, it varies based on two factors: the proximity between the CO2 processing plant and the delivery point.
It's important to note that transportation costs account for a significant portion of the CO2 price.
The other factor is the packaging method of CO2. Between storage in bottles and spheres and storage in a tank or external reserve, it's not uncommon to observe a price difference of up to a factor of 10 between the first two and the last. This price variation is explained by the additional steps required for individualized CO2 packaging and the handling involved during deliveries.
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How does supercritical CO2 technology work?
To obtain supercritical CO2, it is necessary to heat and pressurize carbon dioxide. This supercritical phase is achieved starting at 31°C and 74 bars of pressure. However, to meet the needs of various applications using supercritical CO2, Dense Fluid Degreasing machines typically operate between 35 and 50°C with an equivalent pressure range of 150 to 300 bars.

Both pressure and temperature parameters have an impact on the density of CO2 and its ability to dissolve fats or other types of molecules. The first level of "best solvent power" of supercritical CO2 is achieved at 35°C and 150 bars of pressure. At this stage, the density of CO2 is the highest, around 0.86, which is close to that of water. The second level is achieved at 50°C and 300 bars of pressure, again resulting in the high density of supercritical CO2 and improved solvent power.

It's worth noting that, unlike other cleaning or extraction processes, the processing temperatures with supercritical CO2 are relatively low. It's also important to maintain a balance between pressure and temperature to preserve the solvent power of supercritical CO2.
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Does supercritical CO2 pose any risks?
The main risk associated with the use of CO2 is the risk of anoxia, which is the displacement of oxygen in the air by another gas, such as CO2. Naturally, Dense Fluid Degreasing machines are equipped to prevent this risk:
  • Our equipment is equipped with protective enclosures. These enclosures serve both to protect the machine's equipment and to facilitate the removal of CO2 in case of a leak.
  • Safety standards governing the use of CO2 require the installation of CO2 sensors. One sensor is connected to the autoclave unit, and the other is positioned in the room where the machine is installed.
Specific Case: Installation of a supercritical CO2 cleaning machine in a cleanroom: In the case of using a Dense Fluid Degreasing machine in a cleanroom, the ventilation must be powerful enough to ensure the evacuation of CO2 in addition to the other airflows it must manage. Since CO2 is neither flammable nor explosive, machines using supercritical CO2 are not classified as ATEX equipment. However, our equipment, which includes pressurized components, is subject to specific standards such as the PED (Pressure Equipment Directive). This standard requires periodic inspections of these components, which can be integrated into the preventive maintenance actions carried out by the Dense Fluid Degreasing teams. For more information, please refer to the Regulations page.
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