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Sample pretreatment method, halogen content detection method and application

A sample pretreatment and detection method technology, applied in the field of chemical analysis, can solve problems such as the accuracy of halogen test results to be improved and inaccurate testing, and achieve the effect of increasing accuracy and improving recovery rate

Pending Publication Date: 2021-03-26
广州博诺通技术股份有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, this method can only analyze soluble halides, and insoluble halides cannot be absorbed by the eluent. Therefore, the test is inaccurate in the next step of ion chromatography for quantitative analysis.
And even if one of the problems in the above-mentioned prior art is overcome, the inventor finds that the accuracy of the halogen test results in wastewater still needs to be improved

Method used

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  • Sample pretreatment method, halogen content detection method and application
  • Sample pretreatment method, halogen content detection method and application
  • Sample pretreatment method, halogen content detection method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] 1. Sample weighing: Weigh 0.5000g of the initial sample to be tested into a 50ml volumetric flask, and then add 15ml of potassium iodide aqueous solution to the volumetric flask with a concentration of 30mmol / l. Thoroughly mix the sample with potassium iodide aqueous solution, let it stand for 10 minutes, and transfer it to a 50ml volumetric flask after filtering through a microporous membrane, and dilute to 50ml with an appropriate amount of deionized water to obtain an intermediate sample. Take 10g of the intermediate sample into a 50ml volumetric flask, add 10ml of calcium hydroxide aqueous solution (concentration is 20mmol / L), shake sufficiently to make the fluoride ions in the sample react with calcium ions to form insoluble calcium fluoride precipitates, and dissolve the insoluble calcium fluoride The precipitate was filtered and the hypophosphite was retained. Dilute to 50ml with an appropriate amount of deionized water to obtain a defluorinated sample.

[0082]...

experiment example 1

[0101] According to the detection methods provided in the embodiments and comparative examples of the present invention, waste water is used as an object to detect the content of chloride ions in each sample, and the recovery rate of free halogen and bound halogen in wastewater is calculated using chloride ions as an example. Silver chloride containing free chlorine 1.0mg / L and chlorinated paraffin standard solution containing 1.0mg / L combined chlorine were used for analysis. Record the data in Table 1 and Table 2.

[0102] Table 1 Chloride ion content test result

[0103]

[0104]

[0105] Table 2 Chloride ion recovery test result

[0106]

[0107] The results in Table 1 and Table 2 show that after the samples to be tested are treated with soluble iodide aqueous solution, the content of free chlorine and total chlorine is tested in two steps, and the content of free chlorine and combined chlorine can be obtained respectively. And the recovery rate of the present in...

experiment example 2

[0109] According to the steps provided in the Examples and Comparative Examples, the analysis was carried out using sodium fluoride standard solution containing 1.0 mg / L fluoride ion and sodium hypophosphite standard solution containing 1.0 mg / L hypophosphite.

[0110] Table 3 Fluoride ion content test results

[0111]

[0112] The results in Table 3 show that when the sample contains both fluoride and hypophosphite, the peak times of the two ions are consistent, see figure 1 and figure 2 . Because the software cannot distinguish, what is quantified is the sum of the contents of the two ions, and it is easy to classify the hypophosphite as the fluoride ion. When calcium hydroxide solution is introduced to separate calcium fluoride and calcium hypophosphite through filtration, the content of hypophosphite and fluoride ion can be distinguished, that is, the content of fluoride ion + hypophosphite in the intermediate sample is C1, and the defluoridated sample The measured ...

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Abstract

The invention discloses a sample pretreatment method, a halogen content detection method and application, and relates to the technical field of analytical chemistry. The sample pretreatment method comprises the following steps: reacting a to-be-detected sample with a first iodide aqueous solution to obtain an intermediate sample; reacting the intermediate sample with a calcium hydroxide aqueous solution, and performing filtering to obtain a defluorination sample. The halogen content detection method comprises the following steps: pretreating a sample by adopting the pretreatment method; respectively detecting the ion content in the intermediate sample and the defluorination sample by adopting an ion chromatography method, and subtracting the measured ion content of the peak appearing in the defluorination sample for 2-4 minutes from the measured ion content of the peak appearing in the intermediate sample for 2-4 minutes to obtain the content of fluorine in the sample to be detected. The detection method can avoid inaccurate fluoride ion detection data caused by approximate appearance time and peak shape of hypophosphite ions and fluoride ions when ion chromatography is adopted todetect the ion content; therefore, the method is accurate in detection result and can be applied to detection of halogen content in wastewater.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a sample pretreatment method, a halogen content detection method and an application thereof. Background technique [0002] Industrial wastewater usually contains both inorganic salts of halogen (free halogen) and organic compounds containing halogen (combined halogen). The parameter adjustment and wastewater discharge are particularly important. However, sample pretreatment is the key to the analysis of wastewater samples, which has a great influence on the accuracy of test results, and the recovery rate of halogens is low. Therefore, conventional inorganic acid digestion is not suitable for accurate quantitative analysis of halogens. The current pretreatment techniques for halogen samples mainly include pyrolysis, alkali fusion and oxygen bomb. The pyrolysis method causes the sample to undergo pyrolysis at high temperature to release halogen, which is tested by IC (i...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/34G01N1/44G01N30/96
CPCG01N1/28G01N1/34G01N1/44G01N30/96
Inventor 胡智枫林华端李理钟行李杨锐
Owner 广州博诺通技术股份有限公司
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