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Indirect formaldehyde screening and detection analysis method

An analysis method, formaldehyde technology, applied in the field of detection and analysis of formaldehyde in aqueous solution, can solve the problems of cumbersome operation steps and long time consumption, and achieve the effect of simple mechanism and easy operation

Inactive Publication Date: 2016-11-16
ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] From the perspective of practicability, the present invention overcomes the defects of cumbersome operation steps (derivatization reaction) and time-consuming (at least half an hour) of the prior art, and proposes an indirect screening, detection and analysis method for formaldehyde, using ammonia or Ammonium ions are used as reaction reagents. Under the conditions of alkaline solution and certain reaction temperature, they react quantitatively with formaldehyde in the aqueous solution to generate hexamethylenetetramine, and then directly use electrospray tandem mass spectrometer to conduct the reaction of hexamethylenetetramine. The indirect detection and analysis method of formaldehyde detection, the whole analysis process does not exceed 15 minutes

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  • Indirect formaldehyde screening and detection analysis method

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Embodiment 1

[0042] Embodiment 1: experimental procedure

[0043] The experimental steps of the present invention are as follows, and the conditions are all optimized results. The invention is based on the indirect detection and analysis method of formaldehyde, which is based on ammonia or ammonium ion quantitatively reacting with formaldehyde in aqueous solution to generate hexamethylenetetramine, and then directly adopts an electrospray tandem mass spectrometer to detect the hexamethylenetetramine. Ammonium carbonate ((NH 4 ) 2 CO 3 ) is the reaction reagent as an example to illustrate the experimental procedure for the detection of free formaldehyde in aqueous solution.

[0044] (1) The experimental steps for the reaction of ammonium root and formaldehyde are as follows: first, under the condition of 20°C, prepare a saturated ammonium carbonate solution (solubility in water at 20°C is 100g / 100mL) for use; then take 50 microliters of ammonium carbonate solution for use In 1 ml of fre...

Embodiment 2

[0045] Embodiment 2: the establishment of standard curve:

[0046] Prepare hexamethylenetetramine aqueous solution, the reference concentrations are 0.01, 0.025, 0.05, 0.1, 0.5, 1.0 mg / L;

[0047] (1) The liquid chromatography condition in the liquid chromatography mass spectrometry is: C 18 Column, column diameter 2.1mm, column length 150mm; mobile phase methanol and water (80:20), isocratic elution; flow rate 0.4mL / min; hexamethylenetetramine retention time: 0.96min; Volume: 5 microliters;

[0048] (2) The analysis conditions of the electrospray tandem mass spectrometer in the liquid chromatography mass spectrometer are: MRM mode (multiple ion reaction mode), the parent ion is m / z 141, and the product ions are m / z 112, m / z 98 and m / z 85 (the total ion current chromatogram of the liquid chromatography electrospray tandem mass spectrometer of hexamethylenetetramine is shown in Figure 4 , a chromatographic peak with a retention time of 0.96min; the scanning mass spectrum o...

Embodiment 3

[0052] Example 3: Determination of free and hydrolyzable formaldehyde in textiles

[0053] Reference standard: GB / T 2912.1-2009

[0054] This example shows the case where the sample to be tested is a textile and all accessible parts of the textile sample are tested.

[0055] 1. Sample preparation

[0056] The samples were not conditioned, and the pre-conditioning may affect the formaldehyde content in the samples. The samples were sealed and stored before testing.

[0057] Take two samples from the sample, cut them into pieces, and weigh 1g, accurate to 10mg. If the formaldehyde content is too low, increase the sample size to 2.5 g to obtain satisfactory accuracy.

[0058] 2. Sample extraction and pretreatment

[0059] According to the requirements of GB / T 2912.1-2009, put each sample into a 250mL Erlenmeyer flask with a stopper, add 100mL of water, close the lid tightly, put it in a water bath with a temperature of (40±2)°C, shake (60±5) min, and then filtered into anot...

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Abstract

The invention relates to the field of detection analysis of formaldehyde and discloses an indirect screening and detection analysis method for formaldehyde in a water solution. According to the method, ammonia or ammonium ions are taken as a reaction reagent and rapidly react with formaldehyde under the slightly alkaline pH condition at the certain reaction temperature, hexamethylene tetramine is produced, hexamethylene tetramine in the solution is directly detected with an electrospray ionization tandem mass spectrometer, corresponding qualitative and semiquantitative information of formaldehyde is obtained, and the whole analysis process doesn't exceed 15 min. The method adopts a simple mechanism and is simple, convenient and rapid to operate and suitable for rapid screening and detection of formaldehyde in the water solution.

Description

technical field [0001] The invention relates to the field of detection and analysis of formaldehyde in aqueous solution, in particular to a method for indirect screening, detection and analysis of formaldehyde by using ammonia or ammonium ion as a reaction reagent. Background technique [0002] Formaldehyde (molecular formula HCHO, molecular weight 30.03) is a colorless gas with a pungent smell, easily soluble in water, alcohol and ether, is the simplest and most common aldehyde substance, has a strong pungent smell, slightly heavier than air, Usually its 35%-40% aqueous solution is called formalin, and its boiling point is 19°C. It is a toxic substance with high solubility and strong volatility. Formaldehyde is an important chemical raw material and organic solvent. It is often used in the manufacture of industrial products such as resins, plastics, adhesives, and rubber. It can also be used as a preservative (for food, cosmetics, and wood, etc.). In recent years, with the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 于文佳望秀丽张雅婷卫碧文郑翊
Owner ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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