HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing content of chromium in paper for cigarette
A quantitative analysis, chromium content technology, applied in the direction of analysis of materials, measurement devices, material separation, etc., can solve the problem that the key analysis conditions and interference conditions are far apart, and achieve high sensitivity, low detection limit, good repeatability Effect
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[0058] Example 1
[0059] (1) Instruments and reagents
[0060] Agilent 7700x inductively coupled plasma mass spectrometer (Agilent, USA); 1200 high performance liquid chromatograph (Agilent, USA); SIGMA 3-18K high-speed centrifuge (SIGMA, Germany); SHZ-82 water bath constant temperature oscillator ( Jintan Guowang Experimental Instrument Factory); Milli-Q Integral ultrapure water system (Millipore Corporation, USA).
[0061] Cr(Ⅲ) single element standard stock solution (GBW08614, 1000 mg / L, National Standard Material Research Center); Cr(Ⅵ) single element standard stock solution (GBW(E) 080257, 100 mg / L, National Standard Material Research Center) ); HNO 3 (UP grade); ammonia (UPLC grade); mobile phase NH 4 NO 3 By HNO 3 Mixed with ammonia water; tuning solution (Ce, Co, Li, Mg, Tl, Y, all 1 μg / L, Agilent, USA).
[0062] (2) Instrument conditions
[0063] The high performance liquid chromatography and the inductively coupled plasma mass spectrometer are connected by PEEK tubing, and ...
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[0089] Example 2
[0090] (1) The instrument and reagents are the same as in Example 1.
[0091] (2) The main instrument parameter conditions of the experiment are shown in Table 3 and Table 4:
[0092] Table 3 HPLC conditions
[0093]
[0094] Table 4 ICP-MS working conditions
[0095]
[0096] (3) Sample pretreatment
[0097] Cut the cigarette paper sample into 0.5 cm×0.5 cm size shape. Accurately weigh 1.0 g of the pretreated sample and place it in a 30 mL plastic quantitative bottle, add 20 mL of 30 mmol / L NaOH solution to the quantitative bottle, close the cap tightly and place it in a rotary shaker at 120 r / min Extract at a rate of 1.5 h, and then let it stand for 10 min. Take 3 mL of the extract and filter through a 0.45 μm aqueous filter membrane, discard the initial 1 mL filtrate, and collect the subsequent 0.8 mL filtrate to obtain the initial filtrate. Use 0.2 mol / L HCl solution to adjust the pH of the initial filtrate to 6.5, and perform complexation reaction with 5 mL...
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[0099] Example 3
[0100] (1) The instrument and reagents are the same as in Example 1.
[0101] (2) The main instrument parameters and conditions of the experiment are the same as in Example 1.
[0102] Cut the cigarette paper sample into 0.5 cm×0.5 cm size shape. Accurately weigh 1.0 g of the pretreated sample and place it in a 30 mL plastic quantitative flask, add 15 mL of 50 mmol / L NaOH solution to the quantitative flask, close the cap tightly and place it in a rotary shaker at 150 r / min Extract at a rate of 2 h, and then let it stand for 10 min. Take 3 mL of the extract and filter through a 0.45 μm aqueous filter membrane, discard the initial 1 mL filtrate, and collect the subsequent 1 mL filtrate to obtain the initial filtrate. Use 0.1 mol / L HCl solution to adjust the pH of the initial filtrate to 7.0, which is the HPLC-ICP / MS analysis solution for detecting the content of hexavalent chromium.
[0103] Others are the same as in Example 1. The experimental results show that u...
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