BS ISO 13913:2014 pdf download – Soil quality — Determination of selected phthalates using capillary gas chromatography with mass spectrometric detection (GC/MS).
5.13 Reference solutions for multipoint calibration (see Annex B). Prepare solutions by adequate dilution of the stock solution (5.12) and internal standards (5.9) with ethyl acetate (5.4). Store the solutions in glass bottles at –18 °C, protected from light, and check the concentration at least every three weeks. 5.14 Solution of the internal standards (see Annex B). 5.14.1 Internal standard solution of D4-phthalates. Weigh e.g. 0,1 g of an internal standard phthalate (D4) (5.9) in a 10-ml volumetric flask (6.13) filled with about 5 ml of ethyl acetate (5.4) and bring to volume with ethyl acetate (5.4). Store the solution in a glass bottle at −18 °C. 5.14.2 Solution I internal standard mix. Combine the solutions of the single internal standard phthalates (5.9) e.g. by dilution 1:100 as follows: Transfer with a syringe 0,1 ml (6.15) of each solution into a 10-ml volumetric flask (6.13) filled with about 5 ml of ethyl acetate (5.4). Bring to volume with ethyl acetate. The final concentration of di-n- octylphthalate (D4), di-n-butylphthalate (D4), and di-(2-ethylhexylphthalate) is 100 mg/l in ethyl acetate (5.4). 5.14.3 Solution II internal standard mix. Take from this 1:100 dilution (5.14.2) e.g. 250 µl, transfer into a 250-ml volumetric flask (6.13), filled with 250 ml of ethyl acetate (5.4). The final concentration of di-n-octylphthalate (D4), di-n-butylphthalate (D4), and di-(2- ethylhexylphthalate) is 0,1 mg/l in ethyl acetate (5.4).
6.6 Vacuum device for clean-up, vacubox, extraction box. 6.7 Stainless steel cock, with stainless steel cone or polytetrafluoroethylene (PTFE) cock with Luer connection for separate vacuum connection. 6.8 Glass cartridges, with Luer cone. 6.9 Polytetrafluoroethylene (PTFE) frits, for cartridges, 6 ml. 6.10 Aluminium foil, heated to 400 °C. 6.11 Stainless steel reservoir, for storage of smaller glass apparatus. 6.12 Measuring cylinders, volumes 50 ml and 100 ml. 6.13 Volumetric flasks, volumes 10 ml, 25 ml, and 250 ml. 6.14 Pasteur pipettes, e.g. 2 ml. 6.15 Syringes, 2 µl, 5 µl, 10 µl, 50 µl, 100 µl, and 500 µl, maximum permitted error ±2 %. 6.16 Gas chromatograph, with capillary column, temperature controlled, with mass spectrometric detection. 6.17 Operating gases, for gas chromatography/mass spectrometer of high purity and in accordance with manufacturer’s specifications. 6.18 Fused silica columns, with non-polar stationary phase (see Annex C for examples). Check the quality of the column e.g. by injecting the reference solution (5.13) and ensure that the separation is satisfactory.