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Detection method for hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in plastic product

A technology of hydroxyethylhexahydro-s-triazine and a detection method, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve problems such as matrix interference, poor detection accuracy and reproducibility, and slow detection speed, and reach the detection limit low cost, good reproducibility and fast detection speed

Active Publication Date: 2018-06-19
GUANGZHOU GRG METROLOGY & TEST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The known detection method of triazine substances applied to the detection of hydroxyethyl hexahydro-s-triazine content in plastic products has problems such as slow detection speed, obvious matrix interference, and poor detection accuracy and reproducibility.

Method used

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  • Detection method for hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in plastic product
  • Detection method for hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in plastic product
  • Detection method for hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in plastic product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of detection method of hydroxyethyl hexahydro-s-triazine, sample pretreatment comprises the following steps:

[0038] S1. Take a representative plastic product A, cut it into pieces of 2mm×2mm×2mm, weigh 1.0 g (accurate to 0.1mg) of the sample and put it into a 60mL glass reaction bottle, add 10 mL of methanol, extract for 60 min, ultrasonic temperature 50 ℃, repeat the above operation once, combine the two extracts, and mix well;

[0039] S2. Concentrate to a small amount with a rotary evaporator, slowly blow nitrogen to nearly dryness, and dilute to 1 mL with methanol, and finally filter the extract through a 0.45 μm microporous membrane to obtain the sample to be tested.

[0040] Preparation of the blank sample to be tested: follow the above sample pretreatment steps, without adding plastic products.

[0041] The samples to be tested were detected and analyzed by gas chromatography-mass spectrometry (GC-MS).

[0042] Preparation of standard solution: Accurat...

Embodiment 2

[0053] Embodiment 2 detection result

[0054] (1) The peak extraction of hydroxyethylhexahydro-s-triazine and the selection of qualitative and quantitative ions

[0055] The peak elution time and qualitative and quantitative ions of hydroxyethylhexahydro-s-triazine are shown in Table 1. figure 1 It is the gas chromatogram of hydroxyethyl hexahydro-s-triazine, figure 2 is the mass spectrum of hydroxyethyl hexahydro-s-triazine, from Table 1 data and figure 1 and figure 2 It can be seen that under the above-mentioned optimized gas chromatography-mass spectrometry conditions, hydroxyethyl hexahydro-s-triazine can be well separated within 14 minutes, with symmetrical peak shapes and little matrix interference.

[0056] Table 1 Peak elution time and qualitative and quantitative ions of hydroxyethylhexahydro-s-triazine

[0057] serial number

Substance name

retention timemin

Quantitative ion m / z

Qualitative ion m / z

1

Hydroxyethylhexahydro-s-tri...

Embodiment 3

[0073] A kind of detection method of hydroxyethyl hexahydro-s-triazine, sample pretreatment comprises the following steps:

[0074] S1. Take a representative plastic product B, cut it into pieces of 1mm×1mm×1mm, weigh 2.5 g (accurate to 0.1mg) of the sample and put it into a 60mL glass reaction bottle, add 50 mL of methanol, extract for 120 min, and ultrasonic temperature 70 ℃, repeat the above operation once, combine the two extracts, and mix well;

[0075] S2. Concentrate to a small amount with a rotary evaporator, slowly blow nitrogen to nearly dryness, and dilute to 5 mL with methanol, and finally filter the extract through a 0.45 μm microporous membrane to obtain the sample to be tested.

[0076] Preparation of the blank sample to be tested: follow the above sample pretreatment steps, without adding plastic products.

[0077] Under the optimized method conditions, add standard substances with final concentrations of 0.1 mg / L, 1 mg / L, and 10 mg / L to the blank sample respe...

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Abstract

The invention discloses a detection method for hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in a plastic product. According to the detection method for the hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in the plastic product, methanol ultrasonic extraction is used for pre-treating a sample, and quantitative and qualitative detection is carried out on the hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine by utilizing a gas chromatography-mass spectrometry. The invention establishes an analysis and testing method for determining the hexahydro-1,3,5-tris(hydroxyethyl)-s-triazine in the plastic product by utilizing the gas chromatography-mass spectrometry. The method disclosed by the invention is simple and rapid; methanol is used as an extracting agent and a very good extracting effect can be realized through the ultrasonic extraction; under optimized analysis conditions, a very good chromatographic peak can be obtained within 14min and a very good separation effect can be obtained; the detection limit of gas chromatography-mass spectrometry analysis detection is low; the detection method has good repeatability and high standard recovery rate.

Description

technical field [0001] The invention relates to the field of analysis and detection of triazines, in particular to a detection method of hydroxyethylhexahydro-s-triazine in plastic products. Background technique [0002] Hydroxyethylhexahydro-s-triazine is a light yellow transparent viscous liquid, soluble in water, easily soluble in methanol, ethanol, acetone and other organic solvents. As an important bactericidal preservative, it is widely used in many fields such as papermaking, coatings, metal processing fluids, adhesives, industrial additives, polymer dispersants and lubricants. Although it has good chemical properties, studies have confirmed that it can cause severe skin burns and eye damage, long-term or repeated exposure can easily cause organ damage, and may cause genetic defects. Because of its persistent, bioaccumulative and toxic hazards, it has attracted great attention from all walks of life. According to the proposal of the Norwegian Environmental Protection...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王华李支薇严洪连林炼锋
Owner GUANGZHOU GRG METROLOGY & TEST CO LTD
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