ISO 18219-2-2021 pdf download.Leather一Determination of chlorinated hydrocarbons in leather – Part 2: Chromatographic method for middle-chain chlorinated paraffins (MCCPs).
WeIgh (0.5 a 0,001) g test leather sample with the analytical babncc (5.1) into the scalable vcscl (52).
Acid 9,9 ml n-hexane (6.1) and 100 p1 internal standard (6.2) and seal the vessel. Extract the sample at
(60 t 5) C in an ultrasonic bath (53) for (60 t 2) mm. Cool down to room temperature (less than 27 CC).
8.3 Sulfunc acid clean-up
Add a S ml aliquo of the extracted hexane solution to a light seaLable vessel (12) and add 1 nil sulfuric acId (6.4). Shake the vessel (5.7) for 10 min Alter separating of the phases (optionally with centnlugatlon). I ml of the hexane phase shall be taken for analysis.
8.4 GC-ECNI-MS Determination
The solution is analysed using GC.ECNI.MS (5.6). An example ala suitable GC.ECNI-MS method Is gwen in AnnexA,
9 Expression of results
9.1 Evaluation
The peak shape evaluation (PSE) have been successfully tested and used. The integration shall be done with PSE. In accordance with examples In AnnnL.
Peak areas from the four quantification masses of the standard are summed up and equated with standard concentration. Peak areas of the samples are summed up too and the concentration is calculated with the response of the standard.
To check the linearity of the analytical system, a calibration standard as reterence standard is analysed alter each ten samples and at the end of the sequence. The deviation In reference to the calibration standard should be within ± 20%, otherwIse the analytical system has to be checked before retrying the analysis.
Sample extract should always be diluted in the concentration range olihe standard. The integration of the samples shall only be done in the retention time window of the standard,
9.2 Ions used for quantification
TabIeA.1 lists the ions used for the quantifIcatIon of MCCPs and the ions used lot the Internal standard llndane,
Sum up the quantifier peak areas from the standard and equate with the standard concentration. Also sum up the quantifier peak areas of the sample and calculate he concentration with responses of the caLibration standards.
To get a quantitative result, each peak area of the extract chrmnatogram has to be below the highest caLibration point. If not, dilute the extract with IS solution (11,2) in the range or specify that the result as bigger than the c.ikt,Lue result
9.3 Interference to MCCPs determination
Quantifier rn/i (mass-to-charge ratio) Ions 431 and 445 shall be quantified only it their area Is above
10% of the quantifier in/s Ions 403 or 417 and the masses are not different (peak shape evaluation), see
C3 and Figure (.3.
C1,(1, quantifier (rn/s 445) shows very low response and an overlay with S(CPs ions, therefore areas should be rejected if Interference from S(XPs Is noticed.ISO 18219-2 pdf download.