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Testing apparatus in DIN EN ISO 11890-2 (Paints and varnishes - Determination of VOC and SVOC contents)
Posted Date:2025/7/22
6 Apparatus
6.1 Gas chromatograph
All of the instrumental parts coming into contact with the test sample shall be made of a material (e.g.glass) which is resistant to the sample and will not change it chemically.
Use one of the two types specified in 6.1.1 and 6.1.2.
6.1.1 Hot-injection system(preferred system)
The instrument shall have a variable-temperature injection block with sample splitter. The injection temperature shall be capable of being set to an accuracy of 1 ℃. Standard operating temperature shall be between 250℃ and 280℃.
NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low volatility and/or high polarity.
6.1.2 Cold-injection system (programmed temperature vaporizer, PTV)
The cold-injection system shall be provided with temperature programming for heating from ambient to 300 ℃ including a sample splitter for split operation.
NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low volatility and/or high polarity.
6.1.3 Selection of sample injection system
The choice between hot-injection and cold-injection will depend on the type of product under test, it is preferred to use the cold-injection system for products which, at high temperature, release substances which interfere with the determination, Cleavage products of binders or additives can be reduced by the use of cold injection system.
Indications of cleavage or decomposition reactions can be obtained by looking for changes in the chromatogram (for example the occurrence of foreign peaks or an increase or decrease in peak size) at various sample injector temperatures (see Annex B).
6.2 Oven
The oven shall be capable of being heated between 40 ℃ and 300 ℃ both isothermally and under programmed temperature control, It shall be possible to set the oven temperature to within 1 ℃, The final temperature of the temperature programme shall not exceed the maximum operating temperature of the capillary column (see 6.4).
6.3 Detector
The following two detectors shall be used.
6.3.1 Mass spectrometer or other mass-selective detector (MS or MSD), for the identification ofV0C and SVOC compounds. To prevent condensation, the detector temperature shall be at least 10 ℃ above the maximum oven temperature.
6.3.2 Flame ionization detector (FlD), for quantification of VOC and SVOC compounds operated at temperatures between 230 ℃ and 300 ℃, To prevent condensation, the detector temperature shall beat least 10 ℃ above the maximum oven temperature. The detector gas supply, injection volume, split ratio and gain setting shall be optimized so that the signals peak areas) used for the calculation are proportional to the amount of substance.
6.4 Capillary column
The column shall be made of glass or fused silica, Columns of sufficient length to resolve volatiles and of maximum internal diameter 0.32 mm, coated with 5 % phenyl-modified poly(dimethylsiloxane) or 6 %(cyanopropyl-phenyl)-methylpolysiloxane at a suitable film thickness shall be used.
NOTE Columns such as DB-5, HP-5,or DB-1301 are suitable1,DB-5, HP-5 or DB-1301 are GC columns characterized as equivalent to USP phase G27 or G43. 0ther columns equivalent USP phase G27 or G43, which meet the pre-set performance criteria of this method can be used as well.
6.5 Analytical system performance criteria
The analytical system performance criteria shall be demonstrated, The limit of quantification (LOQ)for the VOC content and SVOC content, respectively, is 0.01 % by mass. For single compounds, the LOQ is assumed to be 0.005 % by mass using the response factor for diethyladipate (i.e. in DEA equivalents)
NOTE The limit of quantification can deviate for single compounds, If necessary, the compound specific limit of quantification can be determined for the considered single compound(s).
Chromatographic resolution shall be sufficient to separate the compounds DEA and tetradecane (C14)as well as docosane (C22) and dibutylsebacate (DBS). At least a resolution of 1 shall be reached.
For the quantification of VOC content and/or SVOC content at concentrations below 0.1 % by mass the LOQ of triethylene glycol (TEG) shall be proven to be at least 0.005 % by mass, based on the sample weight.
6.6 Qualitative-analysis equipment
If the separated components are to be identified by a mass-selective detector, the instrument shall be coupled to the gas chromatograph.
6.7 Injection syringe
The injection syringe shall have a capacity of at least twice the volume of the sample to be injected into the gas chromatograph.
6.8 Data processing
A suitable software shall be used for integration, calibration, quantification and other data handling processes.
6.9 Sample vials
Use vials made of chemically inert material (e.g. glass) which can be sealed with a suitable septum cap[e.g. a rubber membrane coated with poly(tetra fluoro ethylene)].
6.10 Gas filters
Filters shall be installed in the gas chromatograph connection pipes to adsorb residual impurities in the gases (6.11).
6.11 Gases
6.11.1 Carrier gas, dry, oxygen-free helium, nitrogen or hydrogen, having a purity of at least 99.996 % by volume.
6.11.2 Detector gases, hydrogen having a purity of at least 99,999 % by volume and purified or synthetic air, free of organic compounds.
6.11.3 Auxiliary gas, nitrogen or helium of the same quality as the carrier gas.