Method for rapidly detecting arsanilic acid and roxarsone in water sample

A technology for assimilates and water samples, applied in the field of pollutant detection, can solve the problems of high cost of analysis and testing, expensive instruments, and high prices of consumables, and achieve the effect of improving detection capability, improving detection accuracy, and high test accuracy.

Active Publication Date: 2017-01-11
WUHAN UNIV
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Problems solved by technology

Although the detection method combined with instruments can analyze environmental samples more effectively, the price o...

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  • Method for rapidly detecting arsanilic acid and roxarsone in water sample

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Experimental program
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Effect test

Embodiment 1

[0027] Prepare 100 mL of simulated wastewater solution containing arsanic acid at a concentration of 5 μg / L.

[0028] ① Pipette 25 mL of water sample into a quartz reactor with a stopper, put in a stirring magnet for stirring, add 50 μL (1+1) HCl solution to make the solution strongly acidic, pass nitrogen into the quartz reactor for 10 minutes, and remove oxygen Afterwards, the stopper was plugged and sealed, and the reactor was placed under an ultraviolet disinfection lamp for irradiating for 30 minutes. Then take 4mL of the reacted sample into a 10mL sample tube filled with 0.5mL (1+1) hydrochloric acid, shake well, add 0.5mL 5%+5% thiourea+ascorbic acid (m / V), shake well again, After standing for half an hour, use atomic fluorescence detection, the measurement conditions are: the carrier is 5% HCl, the reducing agent is 0.5% KOH-2% KBH 4 , the carrier gas is high-purity argon (purity ≥ 99.999%). The measurement result was 4.019±0.180μg / L, that is, the total arsenic conce...

Embodiment 2

[0032] Prepare 100 mL of simulated wastewater solution containing roxarsone at a concentration of 5 μg / L.

[0033] ①Pipete 25mL of water sample into the quartz reactor with stopper, put it into the stirring magnet for stirring, add 50μL of 6M NaOH solution to make the solution strong alkaline, pass high-purity nitrogen into the quartz reactor for 10min, after deoxygenation , plugged the plug and sealed, and placed the reactor under the ultraviolet disinfection lamp for irradiating for 30 minutes. Then take 4mL of the reacted sample into a 10mL sample tube filled with 0.5mL (1+1) hydrochloric acid, shake well, add 0.5mL 5%+5% thiourea+ascorbic acid (m / V), shake well again, After standing for half an hour, use atomic fluorescence detection, the measurement conditions are: the carrier is 5% HCl, the reducing agent is 0.5% KOH-2% KBH 4 , the carrier gas is high-purity argon (purity ≥ 99.999%). The measurement result was 2.629±0.178μg / L, that is, the total arsenic concentration i...

Embodiment 3

[0037] Prepare 100 mL of mixed simulated wastewater solution containing 0.5 μg / L arkanic acid and 0.5 μg / L roxarsone.

[0038] ①Pipete 25mL water sample into the quartz reactor with stopper, put it into the stirring magnet for stirring, add 50μL of 6M NaOH solution to make the solution strong alkaline, pass nitrogen into the quartz reactor for 10min, after deoxygenation, Plug the stopper and seal it, and place the reactor under an ultraviolet disinfection lamp to irradiate for 120 minutes. Then take 4mL of the reacted sample into a 10mL sample tube filled with 0.5mL (1+1) hydrochloric acid, shake well, add 0.5mL 5%+5% thiourea+ascorbic acid (m / V), shake well again, After standing for half an hour, detect with atomic fluorescence. The measurement results showed that the total arsenic concentration in the water sample was 0.998±0.016μg / L, that is, the total organic arsenic content was 0.998±0.016μg / L.

[0039] ②Pipete 25mL water sample into the quartz reactor with stopper, put...

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Abstract

The invention discloses a method for rapidly detecting arsanilic acid and roxarsone in water sample. The method comprises the following specific steps of: firstly taking three aliquots of identical water samples, respectively adjusting the pH values of the two aliquots of water samples to be strongly acidic or strongly alkali, then pouring the two aliquots of water samples with adjusted pH values into a quartz reactor, leading into inert gas for removing oxygen, switching on an ultraviolet disinfection lamp for irradiation so as to convert organic selenium into inorganic selenium; and after the reaction is finished, detecting inorganic selenium contained in the three aliquots of water samples by adopting an atomic fluorescence spectroscopy, and respectively obtain background value of inorganic selenium, content of arsanilic acid and content of roxarsone in the water samples. The method is simple to operate, good in repeatability, and high in selectivity, the detection limit of the organic selenium can be greatly reduced, the detection precision can be improved, and the detection capability of a laboratory can be effectively promoted; in addition, chemical reagents are common reagents, so that the cost is low, the use amount is small, and the induced secondary pollution is small.

Description

technical field [0001] The invention belongs to the technical field of pollutant detection, and in particular relates to a method for rapidly detecting low-concentration arsanic acid and roxarsone in water samples. Background technique [0002] Since the 1990s in my country, organic arsenic preparations have been widely used in the livestock and poultry breeding industry, mainly for inhibiting pathogenic microorganisms, improving feed utilization to promote the growth of livestock and poultry, and improving the appearance and color of livestock products. The most commonly used organic arsenic feed additives are p-arsanilic acid and roxarsone. However, the utilization rate of these organic arsenic preparations in animals is extremely low, most of the organic arsenic preparations in the feed will directly enter the surface environment around the farm along with animal excrement, and the organic arsenic preparations remaining on the soil surface can pass through Rainwater runo...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N1/28
CPCG01N1/28G01N21/6404
Inventor 徐晶吴峰夏军张翔李进军张利平
Owner WUHAN UNIV
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