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Procedure in EN 14719 (Pulp, paper andboard-Determinationof the DIPN content by solventextraction)
Posted Date:2026/1/20
8 Procedure
8.1 GC-MS analysis
Maintain the same operating conditions of the GC-MS system throughout the measurements of all solutions prepared in Clauses 6 to 7.3.
8.2 Calibration
Inject the calibration standards prepared in 7.1 together with the control standard (7.3) for GC-MS analysis.
Obtain the integrated peak areas of the DIPN and DEN perks. Construct the calibration line by plotting the total peak area ratio of DIP/DEN versus the mass of DIPN (μg) added to the calibration solutions.
NOTE The correlation coefficients of the calibration lines should be 0,996 or better.
The control standard should give a result from the calibration graph within 8 % of the true value.
If the correlation coefficients are less than 0,996 then fresh intermediate standard stock solutions and calibration solutions should be prepared from the original stock solutions.
8.3 Test piece analysis
8.3.1 Test piece extracts
Inject the test piece extracts and blank as prepared in Clauses 6 and 7.2 for GC-MS analysis.
8.3.2 Determination of DIPN
Identify the six DIPN peaks on the basis of the retention time and measure the total peak areas. Also measure the DEN peak area and calculate the DIP/DEN area ratio.
8.4 Evaluation of data
8.4.1 Interferences
No interferences with the DIPN or DEN peaks arising from the extraction procedure have so far been observed using the method and the GC-MS conditions specified in (4.2)
NOTE If DIPN is found in the blank (7.2) it is recommended to check for the source of contamination.
8.4.2 Determination of the DIPN concentration in the test pieces
8.4.2.1 Graphical determination
Read from the calibration graph (see Clause 8) the quantity of DIPN in μg in the test piece extract by interpolation of the total peak area ratios DIPN/DEN to the x-axis.
8.4.2.2 Calculation from the regression parameters
Calculate the regression line equation according to formula (1):
y=a*x+b
where
y is the regression line (peak area ratio);
a is the slope of the regression line in μg
x is the concentration DIP in micrograms;
b is the intercept of the regression line.
Calculate the mass of DIPN (MDIPN) which was extracted from the board according to the formula (2):
where
MDIPN is the mass of DIPN, expressed in micrograms;
y is the regression line (peak area ratio);
b is the intercept of the regression line;
a is the slope of the regression line in μg
Both procedures yield the mass of DIPN in μg in the extract. If the mass of DIPN is higher than the upper range the calibration line, the solution shall be diluted and analysed once again.
NOTE Calculation from the regression line should be the preferred method.
8.4.3 Calculation of the DIPN content in the paper
Calculate the DIPN content in the paper, board or pulp according to formula (3):
where
DIPNcon is the DIPN content, expressed in milligrams per kilograms;
MDIPN is the mass of DIPN, expressed in micrograms;
md is the dry weight of mass of the test piece taken, expressed in grams.
Calculate the mean of the duplicate determinations.