🏭 Volatile organic compounds in emissions

Environmental PN-EN 13649

Overview

STATUS (as of 06.11.2026). PN-EN 13649:2005 — Polish version, published on 28.04.2005, which implemented EN 13649:2001 [IDT] — has been WITHDRAWN since 08.08.2018; the PKN card does not name a replacing standard and there is no successor in the Polish Standards collection. At European level EN 13649:2001 was superseded by the Technical Specification CEN/TS 13649:2014, which has not been adopted into the PN collection. Despite the withdrawal, the standard has 386 entries in Polish scopes of accreditation at 81 laboratories (copy of the scope database, 06.11.2026) — citing a withdrawn document requires a deliberate decision agreed with the customer.

SCOPE (EN 13649:2001, clause 1). The standard specifies the sampling onto activated carbon, the preparation and the analysis of samples of volatile organic components, e.g. from solvent using processes (a note refers to Directive 1999/13/EC); it can be used as a reference method. The result is the mass concentration (mg/m³) of individual gaseous organic components, in the range from about 0.5 mg/m³ to 2000 mg/m³. For total organic carbon from solvent using processes the standard refers to EN 13526.

PRINCIPLE (clause 4). Three steps: flue gas sampling, treatment of the sampled material and analysis by gas chromatography. Organic components from a measured volume of gas are adsorbed onto activated carbon; interfering particulate matter should be removed and water condensation prevented. The collected material is desorbed with an extraction solvent, an aliquot is injected into a gas chromatograph with a capillary column and an appropriate detector (e.g. flame ionization or mass selective), and evaluated using the calibration function. Desorption efficiency is determined by adding a known amount of reference material to a blank tube; according to a note in the standard it should be better than 80 %.

SAMPLING (clauses 5–6). A system of chemically and physically inert material (a note lists stainless steel, glass, PTFE and polypropylene fluoride as well proven), with a sampling line as short as possible, a filter directly after the probe and protection against condensation. The standard shows examples of sampling without dilution, with dynamic dilution (dilution constant to within 5 %) and with static dilution (bag of inert material in a rigid container; pressure control device not above 250 Pa). The sorbent tube has a main layer of at least 100 mg of activated carbon (e.g. from coconut shell) and a security layer to detect breakthrough; open or used tubes are not reused. Dilution gas — nitrogen or dry air containing less than 0.1 % of the emission limit value of the components investigated. The gas temperature during adsorption should not exceed 40 °C; when the gas is so moist that water condenses, or the concentration risks exceeding the tube capacity, dilution is used. The sample shall represent the process emission and the distribution in the sampling plane; the sampling time is chosen e.g. by the required averaging period and the detection limit.

REAGENTS (5.2). Extraction solvent of chromatographic quality, free from components co-eluting with those of interest; carbon disulfide (CS₂) is suitable for most components from solvent using processes, other solvents for polar substances (Annex B). The chromatograph is calibrated with reference materials corresponding to the process components, prepared in a solution of the extraction solvent; standards should be prepared fresh regularly.

CEN/TS 13649:2014 — WHAT CHANGED. The Technical Specification superseded EN 13649:2001: status changed from standard to Technical Specification, clarified scope, a decision tree for the sampling procedure, sampling strategy aligned with EN 15259, thermal desorption added, and validation information. The solvent-extraction tube has 100 mg of activated carbon in the main layer and 50 mg in the security layer; thermal desorption tubes (stainless steel, inert-coated steel or glass) can be reused. Pump flow — e.g. up to 0.1 l/min for thermal desorption tubes and up to 0.5 l/min for charcoal tubes; thermal desorption is typically three orders of magnitude more sensitive. Liquid water shall not reach the sorbent, and drying tubes (e.g. sodium sulfate) are not used upstream of the sorbent. According to a note in the specification, the limit values of EU Directives are expressed in mg/m³ on a wet basis for non-combustion processes and on a dry basis for combustion, at the reference conditions of 273 K and 101.3 kPa.

REGULATIONS (Poland). Emission standards for installations using organic solvents are set by Chapter 6 of the Regulation of the Minister of Climate of 24 September 2020 on emission standards (Dz.U. 2020 item 1860, § 30–31, Annexes 9–10); it repealed the 2018 regulation (Dz.U. 2018 item 680).

WHAT WE DO NOT GIVE HERE. The minimum sampling time and flow rate of EN 13649 (6.3 onwards), the desorption procedure, chromatographic conditions, calculations and uncertainty — they are outside the available text of both documents. Temperature programmes of the desorber and the chromatograph or trade names of tubes — the sources do not give them.

Method principle

Waste gas is sampled through a filter and a line of inert material, preventing condensation (with dilution if needed), onto an activated carbon tube with a main and a security layer. The organic components are desorbed with an extraction solvent (usually carbon disulfide), an aliquot is analysed by capillary gas chromatography with a detector, for example flame ionization or mass selective, and the concentration is determined from the calibration function taking account of the desorption efficiency. The Technical Specification CEN/TS 13649:2014, which superseded the standard, also allows tubes with sorbents for thermal desorption.

Applications

• Mass concentration of individual gaseous organic compounds in waste gases, e.g. from solvent using processes (EN 13649:2001, clause 1)
• Range from about 0.5 mg/m³ to 2000 mg/m³ (EN 13649:2001, clause 1)
• Installations using organic solvents — VOC emission standards (Poland: Dz.U. 2020 item 1860, Chapter 6)
• Monitoring of individual VOCs according to the requirements of the Industrial Emissions Directive — according to CEN/TS 13649:2014 (clause 1)
• Not for total organic carbon — for it EN 13526 (formerly) and EN 12619 (according to CEN/TS 13649)

Key parameters

Standard

Standard number

PN-EN 13649:2005

Title (PL)

Emisja ze źródeł stacjonarnych — Oznaczanie stężenia masowego indywidualnych gazowych związków organicznych — Metoda z zastosowaniem węgla aktywnego i desorpcji rozpuszczalnikiem

Title (EN)

Stationary source emissions — Determination of the mass concentration of individual gaseous organic compounds — Activated carbon and solvent desorption method

Step-by-step procedure

1. Measurement plan

   Ensure the sample is representative of the process emission and the distribution in the sampling plane; if possible measure under steady operating conditions of the plant (6.1; strategy according to EN 15259 in CEN/TS 13649:2014).

2. Choice of sampling procedure

   Sampling directly onto the sorbent when the gas is not very moist and breakthrough is unlikely; static or dynamic dilution when water condenses or the concentration risks exceeding the tube capacity (6.2).

3. Sampling

   Sample a measured volume of gas through the filter and line without condensation onto a tube with main and security layers; the gas temperature during adsorption should not exceed 40 °C; choose the sampling time according to the averaging period and the detection limit (4.2, 6.2–6.3).

4. Desorption

   Desorb the collected components with the extraction solvent (4.3); according to CEN/TS 13649:2014 alternatively thermal desorption.

5. Desorption efficiency

   Add a known amount of reference material to a blank tube and determine the desorption efficiency (should be better than 80 %) (4.5, Annex B).

6. Analysis

   Inject an aliquot into the chromatograph with a capillary column and an appropriate detector; evaluate using the calibration function prepared from reference materials (4.4, 5.2.3).

7. Calculation and report

   Express the result as the mass concentration of individual components in mg/m³ according to clauses 8–9 of the standard.

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• Carbon disulfide — harmonised CLP classification: H225, H315, H319, H361fd, H372; work under a fume hood, away from ignition sources
• The standard contains no other safety requirements; the rules for working at measurement sites on the stack are set by the laboratory on the basis of a risk assessment

Frequently asked questions