EN 1014-4-2010 pdf download.Wood preservatives – Creosote and creosoted timber – Methods of sampling and analysis – Part 4: Determination of the waterextractable phenols content of creosote.
ultraviolet detector capable of being set at an absorption wavelength of 276 nm;
– an integrator or potentiometric recorder.
NOTE As an alternative, any other HPLC configuration giving at least the same resolution (see Annex A) could be used,
5.4 Analytical balance, capable of weighing to 0.1 mg.
5.5 Laboratory balance, capable of weighing to 0,1 g.
5.6 Brown glass storage flasks, of 100 ml capacity. fitted with ground glass stoppers.
When only very small amounts of creosote (a few grams) are available, the following additional apparatus is necessary.
5.7 Glass screw-topped phial of 10 ml capacity.
5.8 Phase separation one-side silicone-treated filter papers. with a diameter of 70 mm1).
5.9 Glass syringe of I ml capacity.
6 Preparation of the calibration solutions and of the test samples
6.1 Preparation of calibration solutions
Transfer by pipette (5.2) 25 ml, 10 ml and 5 ml of the standard phenols solution (4.18) to a series of 100 ml one-mark volumetric flasks. Make up to the mark with HPLC eluent (4.17).
Transfer the calibration solutions to brown glass storage flasks (5.6). Store the flasks in the dark below 10. C.
The calibration solutions should be prepared each day.
6.2 Preparation of the test sample
6.2.1 General
Prepare duplicate test samples. Ensure that the sample of creosote consists of a single phase. If the laboratory sample derives from creosote in which crystals appear at ambient temperatures, heat the sample to a temperature at which it forms a single phase.
6.2.2 Preparation of 1arge” test samples
NOTE 1 This procedure should be followed if a sufficient amount of creosote (e.g. 250 g) Is available
Weigh accurately and directly into a 500 ml separating funnel 100,0 g to within I mg of the creosote sample. Add the same amount of water (4.2) weighed to an accuracy of 0.1 g. Stopper the funnel and agitate It vigorously for 15 mm. venting the funnel from time to time. Allow to stand until the two layers separate (approximately 10 mm). Filter the aqueous layer through a filter paper until it is clear,
NOTE 2 Several passes through the filter paper may be required.
Weigh 5,0 g of the clear aqueous extract to an accuracy of 0.01 g into a 10 ml one-mark volumetric
flask. Make up to the mark with water (4.2) to produce the test sample.
NOTE 3 It may be necessary to use a larger quantity of the clear aqueous extract if the phenolic content is very low.
6.2.3 Preparation of “small” test samples
NOTE This procedure should be followed in case only a small amount of creosote (e.g. 29 to 5g) is available.
Weigh accurately and directly into the screw-topped phial (5.7) 1 g of the creosote sample to an accuracy of
1 mg. Add twice this amount of water (4.2), weighed to an accuracy of 0,02 g, agitate vigorously for
15 mm.
Filter on the phase separation filter (5.8).
Take approximately 1 ml of the aqueous phase retained on the filter with the syringe (5.9), taking care not to include any creosote.
10 Precision
NOTE The precision data are derived from an inter-laboratory test with 9arg& test samples (6.2.1). The modifications
introduced for small test samples (6.2.2) imply that the precision might be lower than given in 10.1 and 102.
10.1 Repeatability
Duplicate results obtained by the same operator shall be considered suspect if they differ by more than 5 % of the smaller.
10.2 Reproducibility
Single results obtained by two laboratories shall be considered suspect if they differ by more than 15 % of the smaller.
11 Test report
The test report shall include at least the following information:
a) the number and date of this European Standard;
b) full identification of the sample tested and details of Its preparation for analysis;
C) the date of the test;
d) the results of the analysis expressed as grams of water-extractabte phenols per kilogram of creosote (see Clause 9);
e) whether the repeatability has been verified;
f) any particular points observed in the course of the test;
g) any operations not specified in the method or regarded as optional Which might have affected the results.EN 1014-4-2010 pdf download.