Method for detecting content of sulfate in citric acid sample
A sulfate and citric acid technology, applied in the measurement of color/spectral characteristics, etc., can solve the problems of large detection deviation, little production guidance, and inability to detect sulfate content data, etc., to achieve the effect of convenient operation and fast detection.
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[0028] 1) Preparation of reagents
[0029] Sulfate standard solution (0.1mg / mL): Prepared according to GB / T602-2002 (Preparation of standard solutions for the determination of impurities in chemical reagents).
[0030] Stabilizer solution: Glycerin-ethanol mixture (the volume ratio of the two is 1:2): Prepared according to GB1897-2008 (food additive hydrochloric acid).
[0031] Barium chloride solution (250g / L): Weigh 25g of barium chloride, dissolve in water, transfer to a 100mL volumetric flask, add water to make up to the mark.
[0032] Hydrochloric acid solution (3mol / L): Prepared according to GB / T601-2016 (Preparation of Standard Titration Solutions of Chemical Reagents).
[0033] Distilled water: Prepared according to GB / T601-2016-2016 (Preparation of Chemical Reagent Standard Titration Solutions).
Embodiment 1
[0035] This example is used to illustrate the method reproducibility and accuracy of the present invention.
[0036] (1) Move into sulfate standard solution (0.1mg / mL) in six 50ml colorimetric tubes with stoppers respectively; 1mL, 1.5mL, 2.0mL, 2.5mL, the corresponding sulfate mass is 0mg, 0.05mg, 0.10mg, 0.15mg, 0.20mg, 0.25mg;
[0037] (2) Add water to 6 stoppered colorimetric tubes to 15ml, then add 1mL hydrochloric acid solution, 2.5mL stabilizer solution, 1mL barium chloride solution, shake well, dilute to the mark with water to 25mL, 6 stoppered colorimetric tubes The sulfate content in the color tube is 0mg / mL, 0.002mg / mL, 0.004mg / mL, 0.006mg / mL, 0.008mg / mL, 0.01mg / mL, after shaking well, place it in a water bath at 36℃, keep warm 10min;
[0038](3) Detect the absorbance at a wavelength of 420nm, and calibrate the zero point with the absorbance of the blank solution (the standard solution to be tested with a sulfate radical content of 0 mg / mL). See Table 1 below;
...
Embodiment 2
[0045] This example is used to illustrate the application of the method of the present invention in the detection of sulfate content in citric acid samples.
[0046] Carry out experiment according to the method for the step (5)-(7) of embodiment 1, difference is, in step (5), put into the citric acid sample of different batches (known Sulfate standard content in the citric acid sample), use the standard curve that embodiment 1 draws and the linear regression equation that obtains to calculate the content of sulfate in the sample test solution.
[0047] The results are shown in Table 3 below.
[0048] Table 1
[0049] Numbering Sulfate standard solution (mL) Sulfate content (mg / mL) Absorbance (A) 1 0 0 0 2 0.5 0.002 0.053 3 1.0 0.004 0.105 4 1.5 0.006 0.148 5 2.0 0.008 0.198 6 2.5 0.01 0.255
[0050] Y=0.0399X-0.00005, R 2 =0.9988, formula (1);
[0051] Wherein, Y is sulfate radical content;
[0052] X is absorb...
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