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Detection method for special fire retardant content in textile

A detection method and flame retardant technology, which are applied in the detection field of flame retardants

Active Publication Date: 2011-11-16
郭会清
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in gas chromatographic analysis, it often happens that interferences and analytes have the same retention time on the same chromatographic column, especially for samples with unknown pollutants, it is more likely to cause false positives
The national standard GB / T24279-2009 "Determination of Prohibited / Restricted Flame Retardants in Textiles" uses GC-MS detection method and ultrasonic method to extract the target substance in solid samples, which may easily cause problems such as low recovery rate for samples with less content , the lower limit of TEPA determination is 50 mg / kg, and the lower limit of the determination of TEPA, which is prohibited to be used, is too high and needs to be further improved

Method used

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  • Detection method for special fire retardant content in textile
  • Detection method for special fire retardant content in textile
  • Detection method for special fire retardant content in textile

Examples

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Effect test

Embodiment 1

[0059] Example 1. Optimization and selection of parameters when gas chromatography-mass spectrometer measures

[0060] In order to obtain suitable gas chromatography-mass spectrometry parameters, screen and optimize instrument parameters:

[0061] Instruments used: GC-MS 2010plus gas chromatography-mass spectrometry (SHIMAZU, Japan), equipped with AOC20i+s autosampler, Rxi-5MS quartz capillary column, 30 m × 0.25 mm (i.d.) × 0.25 mm, or equivalent;

[0062] (1) Optimization of the inlet temperature

[0063] Select different inlet temperatures, and observe the change of the chromatographic peak area of ​​each target compound (see figure 1 ), the results showed that for TEPA, as the inlet temperature increased, the chromatographic peak area of ​​the TEPA target compound reached the highest point at 220 °C, and then the peak area decreased slightly and tended to be flat. Therefore, the inlet temperature selected in the present invention is 220°C.

[0064] (2) Optimizat...

Embodiment 2

[0077] Example 2: The detection method of tri-[aziridine]-phosphine oxide content in textiles comprises the following steps:

[0078] (1) Sample preparation

[0079] Take 5.0 ~ 10.0 g of cotton fabric sample, cut it to less than 0.5 cm × 0.5 cm, and mix well;

[0080] (2) Sample extraction

[0081] Weigh 1.00 g of the above-mentioned cotton fabric sample and place it in a 5 mL extraction tank, extract it with a fast solvent extraction apparatus, the extraction agent is a mixture of n-hexane and acetone, the volume ratio of the two is 7:3, and the extraction temperature is 60 °C , the pressure was 10.34 MPa, static extraction was performed for 5 min, and each sample was extracted 3 times cyclically. After each extraction, it was washed with 60% of the extraction solvent of the extraction cell volume, and finally purged with nitrogen, and the extraction solution was collected in a 60 mL belt. Transfer the collected extraction solution to a 125 mL chicken heart bottle in a co...

Embodiment 3

[0111] Example 3: Establishment of linear relationship in the detection of tris-[aziridine]-phosphine oxide content in textiles:

[0112] Using the method in Example 2, use the TEPA standard solution diluted with blank matrix solution for GC-MS analysis, the prepared concentrations are: 1 mg / L, 4 mg / L, 10 mg / L, 20 mg / L, 30 mg / L, the determination results were analyzed by the workstation software, the determination linear range was 1-100 mg / L, and the detection limit LOD was 1 mg / L. Take cotton fabric as an example, get the standard curve spectrogram see Figure 7 , the abscissa in the figure indicates concentration (mg / L), and the ordinate indicates (peak area). For actual samples, the lower limit of determination LOQ is less than 4 mg / L. Under the experimental conditions determined by this method, the linear equations and correlation coefficients of other matrices are shown in Table 4 (where Y is the peak area; X is the concentration of TEPA, mg / L). The results showed th...

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Abstract

The invention relates to a detection method for a content of a special fire retardant tris (1-aziridinyl) phosphine oxide (TEPA) in textile. The method comprises steps of sample extracting, detection and identification through gas chromatography-mass spectrum, a blank assay, detection of TEPA content, and the like. A mixture comprising n-hexane and acetone is adopted as an extractant during extracting. The method is characterized in that: the resulting extracting solution is subjected to rotary evaporation, concentration and volume metering, and then is subjected to detecting and identifying through a gas chromatography-mass spectrometer; then a external standard method is adopted for quantitation; a standard working solution having a concentration approaching the special fire retardant TEPA content in a sample solution requiring the detection is selected for the detection through the gas chromatography-mass spectrometer according to the special fire retardant TEPA content in the sample solution requiring the detection. According to the present invention, the method is simple and rapid; the method has high detection precision, a detection lower limit of 4 mg / kg, wherein the detection lower limit of the method is far lower than the detection lower limit of 50 mg / kg in an international standard; recovery rate of the TEPA in the textile can reach 75.22%-99.5%; the method is applicable for detections of various textiles including native fiber and chemical fiber, and the method has wide application scope.

Description

technical field [0001] The invention relates to a method for detecting flame retardants in textiles, in particular to a method for detecting the content of special flame retardant tris-[aziridine]-phosphine oxide in textiles. Background technique [0002] Tris-[aziridinyl]-phosphine oxide, English name: Tris (1-aziridinyl) phosphine oxide or Tris-(aziridinyl)-phosphinoxide (TEPA for short), alias: tris-(1-aziridinyl) Phosphine oxide, CAS No: 545-55-1, molecular formula: C 6 h 12 N 3 OP. TEPA used to be a commonly used special flame retardant for textile materials. It can be used for flame-retardant finishing of polyester and polyester-cotton blended fabrics without harming fibers. Studies have found that long-term contact with these highly toxic flame retardants will have adverse effects on the human body, such as the deterioration of the immune system and reproductive system disorders, hypothyroidism, memory loss and joint stiffness, etc., and later found that it is car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/08
Inventor 王素方郭会清禹建鹰
Owner 郭会清
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