Ion chromatography detection method for negative ions in sodium azide solid product or sodium azide mother liquor

A sodium azide precursor ion chromatography technology, applied in the field of ion chromatography quantitative detection of nitrite ions in sodium azide, achieves the effects of simple and easy operation, accurate and reliable analysis method, and easy popularization

Active Publication Date: 2015-03-11
CHEM TECH ACAD OF SHANDONG PROVINCE
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Problems solved by technology

And adopt ion chromatography of the present invention to realize the separation and detection of inorganic anion in this mother liquor, solve the analysis problem of sodium azide mother liquor, correctly reflect the reaction situation of each raw material in the sodium azide production process, to azide The industrial production of sodium chloride has a very good guiding role and is of great help to the control of product quality

Method used

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  • Ion chromatography detection method for negative ions in sodium azide solid product or sodium azide mother liquor
  • Ion chromatography detection method for negative ions in sodium azide solid product or sodium azide mother liquor
  • Ion chromatography detection method for negative ions in sodium azide solid product or sodium azide mother liquor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 is carried out the partial experiment of screening suitable mobile phase

[0034] 1. Chromatographic conditions

[0035] Ion chromatograph: YC-3000 ion chromatograph;

[0036] Detector: conductivity detection (full scale 30p s / V);

[0037] Chromatographic column: AJS anion chromatographic column;

[0038] The mobile phase is any of the following: 1.2mmol / L sodium carbonate aqueous solution; 2.2mmol / L sodium bicarbonate aqueous solution; 3.1mmol / L sodium carbonate and 1mmol / L sodium bicarbonate aqueous solution (i.e. sodium carbonate and hydrogencarbonate Sodium mixed aqueous solution, in which the concentrations of sodium carbonate and sodium bicarbonate are both 1mmol / L, the same below); 4. 3mmol / L sodium carbonate and 3mmol / L sodium bicarbonate aqueous solution; 5. 1mmol / L sodium carbonate and 2mmol / L Sodium bicarbonate aqueous solution; 6. 2mmol / L sodium carbonate and 1mmol / L sodium bicarbonate aqueous solution; 7. 2mmol / L sodium carbonate and 2mmol...

Embodiment 2

[0046] Embodiment 2 screens the suitable injection concentration of solid product

[0047] The difficulty in determining sodium nitrite in sodium azide is that the content of sodium nitrite in sodium azide products is below 1%. If the sample injection volume is too small, the peak area of ​​sodium nitrite is too small to be quantitative. If the sample If the injection volume is too large, the separation of sodium azide and sodium nitrite is not good, and the resolution and peak shape cannot meet the quantitative requirements and cannot be quantified. Therefore, choosing an appropriate injection concentration is the key to the detection method.

[0048] The following is the determination method of the sodium azide solid product injection concentration:

[0049] 1. Chromatographic conditions

[0050] Ion chromatograph: YC-3000 ion chromatograph;

[0051] Detector: conductivity detection (full scale 30p s / V);

[0052] Chromatographic column: AJS anion chromatographic colu...

Embodiment 3

[0064] As can be seen from the foregoing examples, when detecting the solid product of sodium azide, the best detection condition of the present invention is:

[0065] Detector: YC-3000 ion chromatograph;

[0066] Detector: conductivity detection (full scale 30p s / V);

[0067] Chromatographic column: AJS anion chromatographic column;

[0068] Mobile phase: 2mmol / l sodium carbonate and 2mmol / l sodium bicarbonate mixed aqueous solution;

[0069] Flow rate: 1.5ml / min;

[0070] Injection volume: 25μl;

[0071] Column temperature: 25°C;

[0072] Sample concentration: 0.4 mg / ml.

[0073] The accuracy inspection experiment was carried out on the above-mentioned optimal detection conditions, the method is as follows:

[0074] 1. Preparation of sodium nitrite standard stock solution:

[0075] Accurately weigh 0.1000g of sodium nitrite (excellent grade, Tianjin Kemiou Chemical Reagent Co., Ltd.) dried in a sulfuric acid dryer for 24 hours in a 1000ml volumetric flask, dilute to v...

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Abstract

The invention discloses an ion chromatography detection method for negative ions in a sodium azide solid product or sodium azide mother liquor. The sodium azide solid product or the sodium azide mother liquor is analyzed by the ion chromatography detection, so that sodium azide and negative ions (the negative ions exist in the form of salt) can be fully separated; meanwhile, the species of the negative ions is judged or / and the content of the negative ions is calculated according to a chromatographic peak out result; a used flowing phase is a mixture aqueous solution of sodium carbonate and sodium hydrogen carbonate. The analysis method is accurate and reliable; the operation is simple, convenient and feasible; the analysis method is easy to popularize; the contents of sodium nitrite in the sodium azide solid product and the mother liquor can be detected, the difficulty in separating sodium azide from sodium nitrite is solved, and an extremely good supplementing effect is achieved on the national standard GB / T26754-2011 Industrial Sodium Azide. Furthermore, multiple negative ion components in the sodium azide mother liquor can be detected, and great guiding significance in industrial production of sodium azide is acheived.

Description

technical field [0001] The invention relates to an ion chromatography detection method for anions in sodium azide solid product or sodium azide mother liquor, in particular to an ion chromatography quantitative detection method for nitrite ions in sodium azide, and belongs to the technical field of chemical detection. Background technique [0002] Sodium azide (also known as sodium azide), molecular formula NaN 3 , colorless hexagonal crystal, easily soluble in water and liquid ammonia, slightly soluble in ethanol, insoluble in ether. It is stable at room temperature and decomposes at high temperature. Sodium azide decomposes to release nitrogen gas, which can be used as raw material of gas generant and explosive. At the same time, it is used in organic synthesis, inorganic and analytical chemistry, and it is also the main component of antihypertensive drugs. The largest market for sodium azide abroad is automotive airbag inflators. [0003] At present, there are two main...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 刘茂玲刘丽秀邢伶纪晓红王立芹唐晓婵魏凤
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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