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False positive test method for N-nitrosoamine in rubber product

A technology of nitrosoamine and rubber products, which is applied in the field of chemical inspection and analysis, can solve the problems of enterprise losses, misjudgments, false positives, etc., and achieve the effect of avoiding major losses

Pending Publication Date: 2020-04-24
大加利(太仓)质量技术检测中心有限公司
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, we need to test the N-nitrosoamines in rubber products. The domestic test method standard is GB / T24153-2009. This method is GC / MS method. The sample product is extracted with methanol ultrasonic, and the extract is concentrated The essence of C18 solid phase extraction column, the sample liquid gas chromatography-mass selective detector (GC-MSD) is used for determination, the full scan detection is used for qualitative, and the selected ion is used for external standard method for quantification, but it is tested according to the method specified in this standard , there may be false positives, resulting in misjudgment, which may bring heavy losses to the enterprise

Method used

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  • False positive test method for N-nitrosoamine in rubber product
  • False positive test method for N-nitrosoamine in rubber product
  • False positive test method for N-nitrosoamine in rubber product

Examples

Experimental program
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Effect test

preparation example Construction

[0068] The preparation of described rough sample comprises:

[0069] After the rubber is shredded, it is mixed with methanol for ultrasonic extraction, and the first extract and the first solid phase are obtained after solid-liquid separation;

[0070] Adding methanol to the first solid phase for extraction, obtaining a second extract after solid-liquid separation, combining the first extract and the second extract to obtain a combined extract;

[0071] Concentrating the combined extracts to obtain a concentrate;

[0072] The concentrated solution was vortexed and then diluted to obtain a crude sample.

Embodiment 1

[0074] Such as Figure 1-Figure 24 As shown, take a brown rubber sample, take a representative sample, cut it into particles with a side length of less than 3mm, mix well, weigh 5.0g, put it in a conical flask, add 30mL of methanol, and place it in an ultrasonic generator Medium ultrasonic extraction for 30min. Transfer the extract into a concentrated bottle, then add 20mL of methanol to the Erlenmeyer flask, repeat the extraction once, and combine the extracts. Place the concentrated bottle on a rotary evaporator, control the vacuum at 21.3kPa-16.3kPa, and slowly concentrate in a water bath at 35°C to a little less than 4.5mL. Remove the concentrated bottle, fully rotate and shake on the vortex mixer for 1min, and then transfer the sample liquid in the concentrated bottle into a 5mL brown volumetric flask. Take another 0.5mL methanol to rinse the wall of the concentrating bottle, fully rotate and oscillate on the vortex mixer for 1min, then transfer to a volumetric flask to...

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Abstract

The invention discloses a false positive test method for N-nitrosoamine in a rubber product, which comprises the steps of preparing a sample into a sample solution, and identifying by adopting liquidchromatography or gas chromatography / mass spectrometry. The invention successfully develops a method for identifying false positive during N-nitrosoamine testing, and the identification of false positive can be realized by adopting liquid chromatography or changing GC / MS testing conditions, so that great loss caused by misjudgment of false positive is avoided.

Description

technical field [0001] The invention relates to the technical field of chemical inspection and analysis, in particular to a false positive test method for N-nitrosoamine in rubber products. Background technique [0002] Rubber products are widely used in various fields such as national defense, industry and agriculture, and service industries, and are often used in people's daily life. From pressure cooker gaskets in the food field, sealing gaskets for various glass bottle caps, suction rubber tubes for the production of various liquid condiments, etc., rubber shoes, latex gloves, hot water bags, sports balls, etc. involved in daily necessities, children Utensils such as baby pacifiers, suction nozzles, etc., rubber products abound. The impact of rubber products, especially household rubber products that are in direct contact with the human body, on health has become the focus of people's attention. Research on the possible toxic and harmful substances, especially the highl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 姜文良陆杰祝婉婉高怡梅李丹纪委尹晓雨杨俊益张萌张心欢
Owner 大加利(太仓)质量技术检测中心有限公司
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