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Pretreatment method of polybrominated biphenyls and poly brominated diphenyl ethers in nylon resin and nylon resin products

A polybrominated diphenyl ether and polybrominated biphenyl technology, applied in the field of analytical chemistry, can solve the problems of high solvent consumption, low recovery rate and high extraction temperature, and achieve the effect of improving the method recovery rate

Inactive Publication Date: 2015-12-02
URUMCHI PONY TESTING TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two detection methods both use toluene as a solvent for the pretreatment of polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE), and the method of Soxhlet extraction. Because nylon resin is difficult to dissolve in toluene, these two methods measure The recoveries of PBB and PBDE methods are very low, generally no more than 60%, and consume a lot of solvents, the extraction temperature is too high, and the time is long, which will easily cause some components to decompose under long-term high temperature, making nylon resin and its products data and Harmful substances such as brominated flame retardants in its products cannot be accurately measured

Method used

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  • Pretreatment method of polybrominated biphenyls and poly brominated diphenyl ethers in nylon resin and nylon resin products
  • Pretreatment method of polybrominated biphenyls and poly brominated diphenyl ethers in nylon resin and nylon resin products

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Experimental program
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Effect test

Embodiment 1

[0012] 1. Reagents and equipment:

[0013] Reagents: phenol (analytically pure), toluene (chromatographically pure), methanol (chromatographically pure); materials: 20ml stoppered test tube, filter paper, funnel, 25ml volumetric flask, 5ml graduated pipette, nylon resin sample; instrument: grinder, available Temperature adjustment ultrasonic extraction machine, analytical balance.

[0014] 2. Operation steps:

[0015] (1) Take a representative sample and shred it with scissors to a size of 5 mm. During the crushing process, the sample should be avoided from contamination.

[0016] (2) Grind the chopped samples with a high-speed grinder until the particle size is less than 0.5 mm (cool the samples with liquid nitrogen for 5 minutes if necessary).

[0017] (3) Accurately weigh two parallel samples that are uniformly crushed, 0.1 g (accurate to 0.1 mg) of each sample, and place them in two 20 ml stoppered test tubes respectively.

[0018] (4) Place the phenol reagent bottle in...

Embodiment 2

[0023] Add decabromobiphenyl and decabromodiphenyl ether to the negative nylon resin particles where polybrominated biphenyls and polybrominated diphenyl ethers are not detected, so that the theoretical spiked concentrations in the sample are: 25.0mg / kg, 50.0mg / kg, 100.0 mg / kg, according to the above sample pretreatment method and instrumental analysis detection method to carry out the experiment. The sample of each spiked concentration was measured in parallel three times, and the average value of the three measurements was taken. According to the amount of reagent added and the measured results, the spiked recovery rate of the sample was calculated. The experimental results are shown in Table 1. It can be seen from Table 1 that the recovery rate of the sample addition is between 92-100%. The detection recovery and analytical precision fully meet the experimental requirements.

[0024] Table 1 The recovery rate of standard addition of nylon resin

[0025]

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Abstract

The invention belongs to the field of analytic chemistry, and relates to a pretreatment method of polybrominated biphenyls and poly brominated diphenyl ethers in nylon resin and nylon resin products. In hazardous substance determination of nylon resin, especially brominated flame retardant determination, flame retardant recovery rate obtained via a standard pretreatment method is extremely low because of the properties of nylon resin; Soxhlet extraction recovery rate in eight hours is lower than 70%; and recovery rate of conventional ultrasonic extraction is even lower. The pretreatment method is capable of reducing sample pretreatment time to about 30min, and recovery rate is 93% or higher. The pretreatment method is simple and convenient; both labour and time are saved; and environmental protection is realized.

Description

Technical field: [0001] The invention belongs to the field of analytical chemistry, and relates to a pretreatment method for polybrominated biphenyls and polybrominated diphenyl ethers in nylon resins and products thereof, in particular to an innovative invention of an extraction technology for detecting the content of polybrominated biphenyls and polybrominated diphenyl ethers in nylon resins and products thereof. Background technique: [0002] Detection of brominated flame retardants in electronic products, especially polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE). The methods used often include the International Electrotechnical Commission method IEC62321: 2008 "Electrical and Electronic Products - Determination of the Concentration of Six Restricted Substances" and the national standard GB / Z21276-2007 "Restricted Substances in Electrical and Electronic Products Polybrominated Biphenyls (PBBs), PBDEs (PBDEs) detection method" method. These two d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 宋薇潘星科
Owner URUMCHI PONY TESTING TECH CO LTD
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