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Method for detecting caprolactam in chinlon textile

A caprolactam and detection method technology, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of impurities and matrix spectral interference, low response and sensitivity, and poor detector targeting, so as to eliminate matrix and impurities. Accurate and precise results

Active Publication Date: 2016-05-04
JIANGSU ASIA SPACE TESTING TECH SERVICE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both of these two methods have certain limitations. When using HPLC-UV analysis, they are susceptible to spectral interference from impurities and matrix, resulting in false positives and misjudgments.
Analyzed by gas chromatography, the baseline fluctuates greatly, the noise is high, the detection limit is high, the detector is poorly targeted and the response and sensitivity are low

Method used

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  • Method for detecting caprolactam in chinlon textile
  • Method for detecting caprolactam in chinlon textile
  • Method for detecting caprolactam in chinlon textile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] see Figure 1-4 . The invention discloses the drawing of the standard working curve of caprolactam, using an electronic balance of 1 / 10,000 to weigh 0.0817g caprolactam standard product (purity is 98%), put it in a 100mL volumetric flask, dissolve it with methanol and set the volume to the scale line, Shake well to prepare a caprolactam stock solution with a concentration of 800mg / L; then pipette 1000uL of the caprolactam stock solution into a 100mL volumetric flask, dilute to the mark with methanol, and shake well to obtain a caprolactam intermediate solution with a concentration of 8mg / L; Pipette 50uL, 100uL, 200uL, 500uL, and 1000uL caprolactam intermediate solutions into five 100mL volumetric flasks, dilute to the mark with methanol, shake well, and obtain concentrations of 4ug / L, 8ug / L, 16ug / L, 40ug / L, 80ug / L caprolactam standard solution.

[0071] The above-mentioned standard solution was detected with an ultra-high performance liquid chromatography triple quadr...

Embodiment 2

[0075] see Figure 5 . The invention discloses a detection method for caprolactam in women's sweaters (acrylic 72.7%, nylon 27.3%). The nylon textiles are selected, shredded manually, and mixed uniformly. Select a sample with a size of 2mm*2mm, accurately weigh 1.0g of the shredded sample, accurate to 0.0001g, put it in a 40ml reaction tube, add 20.0ml of double distilled water, keep the temperature in an oven at 100°C for 1 hour, and then adjust the temperature at a frequency of Ultrasonic treatment in a 40kHz ultrasonic cleaner for 30min, take it out and cool to room temperature, shake up and down, filter into a clean extraction tube, use a needle syringe to pass the supernatant through a 0.23um water filter membrane to obtain the test solution.

[0076] Repeat the above preparation process of the test solution 3 times to obtain 3 parallel samples A, B and C of the test solution.

[0077] The above three parallel samples were detected with an ultra-high performance liquid ...

Embodiment 3

[0085] see Figure 6 . The invention discloses a method for detecting caprolactam content in supersoft nylon one-piece trousers (56.1% polyester fiber, 31% nylon, and 12.9% spandex). The above-mentioned nylon textiles are selected, shredded manually, and mixed uniformly. Select a sample with a size of 2mm*2mm, accurately weigh 1.0g of the shredded sample, accurate to 0.0001g, put it in a 40ml reaction tube, add 18.0ml of double distilled water, keep the temperature in an oven at 80°C for 90min, and then at a frequency of 40kHz Ultrasonic treatment in an ultrasonic cleaner for 20 minutes, take it out and let it cool to room temperature, shake it up and down, filter it into a clean extraction tube, use a needle syringe to pass the supernatant liquid through a 0.22um water filter membrane, and obtain the test solution.

[0086] Repeat the above preparation process of the test solution 3 times to obtain 3 parallel samples A, B and C of the test solution.

[0087] The above three...

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Abstract

The invention discloses a method for detecting caprolactam in a chinlon textile. The method comprises the following steps: treating the chinlon textile to obtain chinlon textile fragments; weighing a certain quantity of the chinlon textile fragments, adding secondary distilled water, and performing constant-temperature treatment in a drying oven of 80-120 DEG C for 45-90 minutes; performing ultrasonic treatment in an ultrasonic cleaner for 20-50 minutes, taking the fragments out, cooling to the room temperature, shaking uniformly, filtering, extracting supernatant liquid, and filtering through a water-borne filtering film to obtain liquid to be detected; and detecting the content of the chinlon textile in the liquid to be detected by adopting an ultra-high performance liquid chromatography triple quadrupole gas chromatograph-mass spectrometer. According to the method, distilled water ultrasonic extraction is adopted, so that a sample treatment process is simplified, the cost is lowered, and the detection efficiency is increased; a detection limit is 40mumg / kg, which is 10-20 times lower than that of the conventional caprolactam detection method, and the detection demand of future ecological textiles can be met.

Description

technical field [0001] The invention relates to a detection method of caprolactam, in particular to a detection method of caprolactam in nylon textiles. Background technique [0002] Nylon, the scientific name of polyamide fiber, is the general name of polyamide fibers produced in China. Internationally known as nylon. High strength, wear resistance, ranking first among all fibers. Its abrasion resistance is 10 times that of cotton fiber, 10 times that of dry viscose fiber, and 140 times that of wet fiber. It can be purely spun or blended for various clothing and knitwear. There are many varieties of nylon, including nylon 6, nylon 66, nylon 11, and nylon 610. The most important ones are nylon 66 and nylon 6. The properties of various nylons are not exactly the same. The common feature is that there are amide chains on the main chain of the macromolecules, which can absorb water molecules and form a crystal structure. They are excellent in wear resistance and are excellen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 张乐乐朱红娟李明沈祁峰周文静
Owner JIANGSU ASIA SPACE TESTING TECH SERVICE CO LTD
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