SN/T 1599-2005Determination for major elements in coal ash by ICP-AES (English PDF)

3.5 Bisphenol A standard stock solution: accurately weigh 10mg of bisphenol A

standard (3.4); place it in a 100mL volumetric flask; dilute to the mark by acetone (3.1);

and mix well. The concentration of this solution is 100g/L.

3.6 Preparation of standard working solution: respectively pipette appropriate volume

of bisphenol A standard stock solution (3.5); dilute by acetone (3.1) to prepare standard working solution with required concentration.

at 4000 r/min for 15 min in a centrifuge (4.7). Absorb the supernatant by a syringe (4.8);

pass the injecting solution through a 0.20µm organic filter membrane (4.9); and collect the filtrate in a brown bottle. Pipette 1mL of the filtrate to a graduated centrifuge tube accurately; add 100µL of derivatization reagent pentafluoropropionic anhydride (3.3);

place in a vortex mixer (4.10) and vortex to mix; derivatize in a constant temperature water bath (4.11) at 60°C for 30min. After that, place it in a nitrogen blower (4.12) and slowly blow it to near dryness. Add 1mL of n-hexane (3.2); vortex to mix; and transfer the solution to the sample injecting bottle for gas chromatography-mass spectrometry detection.

6.3 Preparation of standard working solution

Accurately transfer a certain volume of standard solution with the appropriate concentration to the graduated centrifuge tube (4.6); add 100µL of the derivatization reagent pentafluoropropionic anhydride (3.3); and follow the 6.2 derivatization procedures below.

6.4 Gas chromatography – mass spectrometry conditions

6.4.1 Chromatographic column: 30m × 0.25mm (inner diameter) × 0.25µm (film

thickness); HP-5MS quartz capillary column or equivalent.

6.4.2 Chromatographic column temperature: initial temperature is 70°C, maintain for

1min; then raise the temperature to 210°C at 30°C/min; and then raise the temperature to 260°C at 10°C/min, and maintain for 2min.

6.4.3 Inlet temperature: 260°C;

6.4.4 Mass spectrometer interface temperature: 280°C;

6.4.5 Carrier gas: helium, purity >=99.99%; flowrate of 1.0mL/min;

6.4.6 Sample injecting method: split-less injection; open the valve after 1.0min;

6.4.7 Sample injecting quantity: 1µL;

6.4.8 Electric ionization method: EI;

6.4.9 Electric ionization energy: 70eV;

6.4.10 Determination method: selective ion monitoring method;

6.4.11 Select monitoring ion (m/z): 265, 505, 520;

6.4.12 Solvent delay time: 5min.

6.5 Gas chromatography – mass spectrometry determination

M – specimen mass, in g.

9.1 Repeatability

In the same laboratory, the same person uses the same equipment, the same test method, and the absolute difference between the two parallel determination results of the same test object within the day is no greater than 10% of the arithmetic mean of the two measured values.

9.2 Reproducibility

In different laboratories, the same person uses the same equipment and the same test method. The absolute difference between two parallel measurements of the same object is no greater than 15% of the arithmetic mean of the two measured values.

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