Instruments and reagents
An AA500 continuous flow analyzer (SEAL, Germany); a SL252 electronic balance (Shanghai mingqiao electronic instrument factory, China); and a Milli-Q ultrapure water meter (Merck millipore, USA) were used. All chemicals used in this work were Analytical-grade and deionized water was used throughout. Hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, chloroform, ethanol, sodium tetraborate, isonicotinic acid and 4-aminoantipyrine were purchased from Sinopharm Chemical Reagent Co., Ltd (China). Triton X-100, sodium hydroxide and potassium chloride were obtained from Tianjin Damao chemical reagent factory (China). Potassium ferricyanide, Sodium nitroprusside, sodium salicylate and N, N-dimethylformamide were supplied by Tianjin Tianli Chemical Reagent Co., Ltd (China). Potassium dihydrogen phosphate, disodium hydrogen phosphate, pyrazolone and methylene blue trihydrate were prepared from Tianjin kemiou Chemical Reagent Co., Ltd (China). Trisodium citrate dehydrate, polyoxyethylene lauryl ether( and sodium dichloroisocyanurate were purchased from Shanghai Aladdin biochemical technology Co., Ltd (China). The standard solutions of volatile phenol, cyanide, anionic surfactant and ammonia nitrogen in water were purchased from China Academy of metrology.
Experimental Procedures
Volatile phenol reagent
Distillation reagent: dilute 160 mL phosphoric acid to 1000 mL with deionized water; Reserve buffer: weigh 9 g boric acid, 5 g sodium hydroxide and 10 g potassium chloride respectively, and dilute to 1000 mL with deionized water; Absorption reagent (updated every week): accurately measure 200mL of reserve buffer, add 1mL of 50% Triton X-100 (V / V, Triton X-100/ ethanol), and use it after filtration with 0.45 um filter membrane; Potassium ferricyanide (updated weekly): weigh 0.15 g of potassium ferricyanide and dissolve it in 200 mL reserve buffer, add 1mL of 50% Triton X-100, and use it after filtration with 0.45 um filter membrane; 4-aminoantipyrine (updated weekly): weigh 0.2 g of 4-aminoantipyrine and dissolve it in 200 mL reserve buffer, add 1 mLof 50% Triton X-100, and use it after filtration with 0.45 um filter membrane.
Cyanide Reagent
Distillation reagent: with volatile phenol; Buffer: weigh 3 g of potassium dihydrogen phosphate, 15 g of disodium hydrogen phosphate and 3 g of trisodium citrate dihydrate in deionized water and dilute to 1000 mL, and then add 2 mL of 50% Triton X-100.Chloramine T: weigh 0.2 g chloramine T and dilute it to 200 mL with deionized water; Chromogenic agent: chromogenic agent A: completely dissolve 1.5 g of pyrazolone into 20 mL of N, N-dimethylformamide; Developer B: dissolve 3.5 g isonicotinic acid and 6 mL 5 mol / L NaOH in 100 mL deionized water. Before use, mix chromogenic agent A and developer B, adjust pH = 7.0 with NaOH solution or HCl solution, then dilute to 200 mL with deionized water and filter for use.
Anionic Surfactant Reagent
Stock buffer: dissolve 10 g sodium tetraborate and 2 g sodium hydroxide in deionized water and dilute to 1000 mL; 0.025% methylene blue solution: dissolve 0.05 g methylene blue trihydrate in deionized water and dilute to 200 mL; Methylene blue stock buffer (updated every day): take 20 mL of 0.025% methylene blue solution and dilute it to 100 mL with stock buffer. Transfer to the separating funnel and wash with 20 mL chloroform, discard the used chloroform and wash again with new chloroform until there is no red in the chloroform layer (usually 3 times), and then filter; Alkaline methylene blue: take 60 mL of filtered methylene blue stock buffer and dilute it to 200 mL with stock buffer, add 20 mL of ethanol, mix evenly and degass; Acid methylene blue: add 2 mL of 0.025% methylene blue solution to about 150 mL of deionized water, add 1.0 mL of 1% H2SO4, and then add it to 200 mL with deionized water. Then add 80 mL of ethanol, mix evenly and degass.
Ammonia Nitrogen Reagent
20% polyoxyethylene lauryl ether solution: weigh 20 g polyoxyethylene lauryl ether and dilute it to 1000 mL with deionized water; Buffer: weigh 20 g trisodium citrate, dilute to 500 mL with deionized water, and add 1.0 mL of 20% polyoxyethylene lauryl ether; Sodium salicylate solution (updated every week): weigh 20 g sodium salicylate and 0.5 g potassium nitrite ferricyanide respectively and dissolve them in 500 mL deionized water; Sodium dichloroisocyanurate solution (updated every week): weigh 10 g sodium hydroxide and 1.5 g sodium dichloroisocyanurate respectively, and dissolve them in 500 mL deionized water.
Preparation Of Standard Series
Volatile phenol and cyanide standards were formulated into 0 µg/L, 2 µg/L, 5 µg/L, 10 µg/L, 25 µg/L, 50 µg/L, 75 µg/L and 100 µg/L with 0.01 mol/L sodium hydroxide solution, respectively. anionic surfactants and ammonia nitrogen standard were prepared with deionized water to 0 µg/L, 10 µg/L, 50 µg/L, 100 µg/L, 250 µg/L, 500 µg/L, 750 µg/L and 1000 µg/L, respectively.
Analysis And Detection
Start the cooling circulation tank, then turn on the computer, the sampler, and the power of the AA500 host in turn, check whether the pipeline is connected correctly, press the air hose into the air valve, cover the peristaltic pump pressure plate, and put the reagent pipeline into pure water. Start the software and activate the corresponding channel window, check whether each connecting tube is connected well, and whether there is looseness and leakage. If there is no liquid leakage, draw the corresponding reagent. After the baseline of the channel window is stable, select and run the set method file for detection and analysis. Instrument conditions are showed in Table 1.
Table 1. Instrument conditions
Analyte
|
Distillation temperature(℃)
|
Heating pool temperature(℃)
|
Sample time(S)
|
Wash time(S)
|
Gain/AUFS
|
Sample /h
|
Sample to wash
|
Colorimetric wavelength(nm)
|
Cyanide
|
145
|
60
|
80
|
100
|
150/0.067
|
20
|
0.8
|
630
|
Volatile phenol
|
155
|
/
|
80
|
100
|
200/0.050
|
20
|
0.8
|
505
|
Anionic surfactant
|
/
|
/
|
80
|
100
|
60/0.167
|
20
|
0.8
|
660
|
Ammonia nitrogen
|
/
|
37
|
80
|
100
|
50/0.200
|
20
|
0.8
|
660
|