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Microemulsion - dimethoxy DBHPF Catalytic spectrophotometric determination of niobium alloys

l / L nitrilotriacetic acid solution, 3.0mL, 5.0 × 10I2mol / L of potassium bromate 1.0mL,[link widoczny dla zalogowanych], non-ionic microemulsion 2.5mL, diluted with water to about 18mL, then add 0.2g / L dimethoxy PF 6.0mL, diluted with water to the mark, shake well. At the same time will release the two colorimetric tubes in boiling water bath, heated 12min accurately removed 4min water cooled to room temperature, with lem cuvette at wavelength of 510nm as the reference fine water and non-catalytic reaction of Catalytic absorbance was A and, and calculate = A. A A value. 3 Results and discussion 3.1 Experimental results show that the absorption curve, non-catalytic system and the catalytic system and the difference between the maximum absorption peaks are in the 510rim △ A place, so choose 510rim for the determination of the wavelength; in the water medium, appeared more than 20rain turbidity, affect the determination result. Microemulsion micelles and water than the sensitivity of the media were increased by 50% and 163%. Therefore, the choice sensitized by microemulsion stability as the media. 3.2 The selection of the acidity of sulfuric acid,[link widoczny dla zalogowanych], 2.0 × 10I2mol/LH: SO the amount in the range of 1.0-2.2mL of its △ A large and stable, so the choice experiment, 2.0mL. 3.3 The results show that the impact of reagent, 5.0 × 10-2mol / L of potassium bromate in the amount of between 0.5 ~ 1.8mL, 1.0 × 10-2mol / L nitrilotriacetic acid solution amount in 2. between 0 ~ 4.5mL, 0.2g / L PF amount of chlorobenzene in the range of 5.0 ~ 6.5mL,[link widoczny dla zalogowanych], non-ionic microemulsion between the amount of the 2.0 ~ 3.0mL, △ A smooth and the maximum, so the choice during the experiment were 1.0,3.0,6.0 and the dosage of 2.5mL. 3.4 Kinetic parameters for the selection of 12min heating time (heating time using a stopwatch control), the linear relationship between reaction time to calculate the regression equation was: △ A = 0.0515t (min) a 0.0033, correlation coefficient r = 0.9996, rate constant K = 8.58 × 10 ~ / s. According to the temperature curve, the regression equation was: l iso = a 4.72 × 10 '× 1 / T + l2.35, the correlation coefficient r = 0.9987, the apparent activation energy: 90.37kl/mol. 3.5 foreign ions and the elimination of 0.4IxgNd (V) / 25mL, the relative error ± 5%, respectively, within the coexistence of these multiple ions do not interfere with: cl one, so: one, Po: a, Na, K ( 1000), ca2, Mg2 (500), Ni Mo (Ⅵ), Zr (Ⅳ), w (V), Se (Ⅳ), Te (Ⅳ), Pd2 (5O), C,, Co2 (1O), Fe n, V (V) (5). 3.6 Working curve, detection and precision of this method with the niobium content in the range 0.4 ~ 20L and showed a good linear relationship, the regression equation: △ A: 0.0598C (C: g / L ) a 0.032, the correlation coefficient r: O. 9993. Do l1 second blank solution measured values, obtained the standard deviation s = 3.07 × 10 one. 3s and work according to the ratio of the slope of the calculated detection limit was 0.15 / L. 3.7 Accurately weigh 0.2500g sample of alloy samples in the platinum dish,[link widoczny dla zalogowanych], add 10mLH: SO3 (1 +2), 5mLHF, 5mLHNO,, low temperature heat to take from the smoke evaporated, cooling, add water to dissolve. Solution was adjusted with NaOH solution, pH5-6 between the separation of iron, filtration, constant volume in the 100mL flask. Determination of the filtrate obtained by experimental methods. The results show that, YSBC11218-94, W-7201 low-alloy steel, Cr38Nil1Nb steel content of niobium (RSD), respectively, 0.312% (1.93%), 0.017% (6.79%) and 0.18% (6.57%), the standard values were 3.11%, 0.018% and 0.19%, the measured results of the method is consistent with the standard value. 20 (14-09-17 Received; 20054) 524 This article is accepted, Dr. Foundation of Shandong Province (No.02BS051)
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