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Method for detecting nitrate ion in iron-containing pickling waste liquid

A nitrate ion and detection method technology is applied in the field of detection of nitrate ions in iron-containing pickling waste liquor, can solve problems such as the interference of impurities in the detection of nitrate ions, and achieves the effects of low cost, accurate measurement and reduced interference.

Inactive Publication Date: 2019-12-06
CHANGZHOU WUJIN YOUBANG WATER PURIFICATION MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is to overcome the defect and deficiency of impurity interference in the detection of nitrate ions in the existing iron-containing waste acid, and to provide a detection method for nitrate ions in iron-containing waste pickling liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of detection method of nitrate ion in iron-containing pickling waste liquid, comprises the steps:

[0033] S1. Take 100ml of prepared iron-containing pickling waste, add soda ash to adjust the pH to 6.5, then add polyacrylamide to flocculate and precipitate to obtain a colorless and transparent supernatant;

[0034] S2. Get the supernatant 50g in a small beaker, add 0.15g reduced zinc powder (the addition of reduced zinc powder is 0.3% of the supernatant quality), the zinc powder specification is 100 mesh, and the purity is 97%. Then dropwise add 4g concentration and be the cadmium chloride solution of 25g / L (the addition of cadmium chloride solution is 8% of supernatant liquid quality), magnetic stirring 5min under 250r / min rotating speed,

[0035] S3. Stand still for 1 min after stirring, take 2.5ml supernatant in a 25ml colorimetric tube, add pure water to dilute to 25ml, add 0.5ml 10g / L p-aminobenzenesulfonic acid solution dropwise, shake well and let stand f...

Embodiment 2

[0038] A kind of assay method of nitrate content in iron-containing pickling waste liquid is basically the same as that of embodiment 1, and difference is: the addition of reduced zinc powder is 0.20g (the addition of reduced zinc powder is 0.4% of supernatant liquid quality ), the specification of zinc powder is 100 mesh, and the purity is 97%.

[0039] The calculated concentration of nitrate ions in the sample is 4.85g / L, and the error of the detection result is 3.0%.

Embodiment 3

[0041] A kind of assay method of nitrate content in iron-containing pickling waste liquid is basically the same as that of embodiment 1, and difference is: the addition of reduced zinc powder is 0.25g (the addition of reduced zinc powder is 0.5% of supernatant liquid quality ), the specification of zinc powder is 100 mesh, and the purity is 97%.

[0042] The calculated concentration of nitrate ion in the sample is 4.91g / L, and the error of the detection result is 1.8%.

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Abstract

The invention discloses a method for detecting the nitrate ion in iron-containing pickling waste liquid. The method comprises the steps of: flocculating and precipitating the iron-containing picklingwaste liquid, separating to obtain transparent supernatant, adding zinc powder and cadmium chloride solution into the supernatant, stirring and mixing uniformly, performing stirring reaction, taking the supernatant to dilute by adding water after reaction solution is standing, adding sulfanilic acid solution, adding naphthalene ethylenediamine hydrochloride solution after mixing uniformly and placing, placing to develop after mixing uniformly, determining the absorbance value by adopting an ultraviolet spectrophotometer, and obtaining the nitrate content by calculation. According to the detection method in the invention, reaction conditions, such as reduced zinc powder, are controlled; the synergy maximization of the detection effect is achieved; interference of impurities, such as co-existing ion, on a detection result is reduced; the detection result error can be controlled below 4.6%; accurate determination of the nitrate ion in the iron-containing pickling waste liquid is realized;operation is simple; the cost is low; complex pre-processing is not required; the detection speed is rapid; and, the method can be widely used for industrial determination.

Description

technical field [0001] The invention relates to the technical field of chemical analysis and detection, in particular to a method for detecting nitrate ions in iron-containing pickling waste liquid. Background technique [0002] A layer of oxide is produced on the surface of stainless steel and alloy steel in the iron and steel industry during processing, which is usually removed by mixed pickling. At present, domestic and foreign manufacturers mostly use mixed pickling containing nitric acid to remove oxides. Pickling with mixed acid containing nitric acid has the advantages of fast pickling speed and not easy to over-pickling, and the steel after pickling maintains a good surface, which cannot be achieved by other pickling. After repeated pickling, the metal ions in the pickling solution increase to a certain concentration, and the acid content drops to a certain percentage, that is, it loses the pickling ability and becomes a waste solution. However, the total acidity i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78G01N21/33
CPCG01N21/33G01N21/78
Inventor 朱松锋居银栋蒋银峰黄莉君陈炎彬朱芬
Owner CHANGZHOU WUJIN YOUBANG WATER PURIFICATION MATERIALS
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