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Method for identifying and quantitatively determining polyamide material by using GC/MS

A technology for quantitative determination of polyamides, applied in material separation, analysis of materials, measurement devices, etc., can solve the problems of complex operating conditions, difficult to characterize polyamide materials, and expensive instruments, and achieve good repeatability, low cost, Simple to use effects

Active Publication Date: 2020-08-14
广东美塑塑料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since 1939, when the DuPont Company of the United States realized industrial production, polyamide materials have been deeply researched and developed by well-known manufacturers at home and abroad due to their good comprehensive properties, and the market has also grown extensively and rapidly. It includes a variety of varieties such as: PA6 , PA66, PA11, PA12, PA46, PA610, PA612, PAl010, etc., as well as semi-aromatic polyamides PA6T, PA9T, PA10T, etc. developed in recent years, but there are not many methods for the analysis and determination of polyamide materials. And there are still deficiencies, such as FTIR infrared method can only be qualitative but not quantitative, and it is difficult to characterize polyamide materials with the same structure and different carbon chain lengths, but it is powerless for complex composite modified polyamide materials, and PY-GC / MS Although qualitative and quantitative, the instrument is expensive and the operating conditions are complicated

Method used

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  • Method for identifying and quantitatively determining polyamide material by using GC/MS
  • Method for identifying and quantitatively determining polyamide material by using GC/MS
  • Method for identifying and quantitatively determining polyamide material by using GC/MS

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Experimental program
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Embodiment 1

[0021] The method for identification and quantitative determination of polyamide materials using GC / MS provided in this embodiment comprises the following steps:

[0022] a) Weigh 0.1-1g polyamide material sample, and decompose the sample completely into diamine hydrochloride and dibasic acid or terephthalic acid monomer through acid solution such as hydrochloric acid under microwave high-temperature reaction conditions, and filter And constant volume, form the first sample solution;

[0023] b) Pipette 0.1-1ml of the first sample solution in step a) into a constant temperature drying oven, evaporate at a low temperature of 80°C to remove excess hydrochloric acid (acid) and water, and form a sample to be dissolved;

[0024] c) redissolving the sample to be dissolved in step b) with a suitable solvent such as ethanol to form a second sample solution, to be tested;

[0025] d) Qualitative and quantitative determination of the second sample solution is carried out by GC / MS using...

Embodiment 2

[0027] Polyamide samples

[0028] Polyhexamethylene adipamide PA66: Medium viscosity resin, Pingdingshan Shenma;

[0029] Polycaprolactam PA6: medium viscous resin, Sinopec Baling Petrochemical;

[0030] Polyhexamethylene terephthalamide PA6T: Mitsui Chemicals CH230N;

[0031] Polynonanediamine terephthalamide PA9T: Japan Kuraray 1402A.GN2200.

[0032] Instruments and reagents

[0033] Precision balance: XS 125A, Puliss;

[0034] Constant temperature drying oven: GHG-9030A, Suzhou Greda;

[0035] Microwave Digestion Apparatus: ETHOS A, Italian Meltstone;

[0036] GC / MS: QP2010 Ultra, Shimadzu Corporation;

[0037] Ultrasonic: LY-100W, Dongguan Liangyuan Ultrasonic Equipment Co., Ltd.

[0038] Hydrochloric acid 36%^38%: AR analytically pure;

[0039] Ethanol: chromatographically pure;

[0040] Deionized water: laboratory grade water;

[0041] Other utensils: commonly used utensils in chemical laboratories.

[0042] Experimental steps:

[0043] a) Weigh about 0.2 g o...

Embodiment 3

[0049] Polyamide samples

[0050] Polyhexamethylene terephthalamide PA6T: Mitsui Chemicals CH230N;

[0051] Polynonanediamine terephthalamide PA9T: Japan Kuraray 1402A.GN2200.

[0052] Instruments and reagents

[0053] Precision balance: XS 125A, Puliss;

[0054] Constant temperature drying oven: GHG-9030A, Suzhou Greda;

[0055] Microwave Digestion Apparatus: ETHOS A, Italian Meltstone;

[0056] GC / MS: QP2010 Ultra, Shimadzu Corporation;

[0057] Ultrasonic: LY-100W, Dongguan Liangyuan Ultrasonic Equipment Co., Ltd.

[0058] Hydrochloric acid 36%^38%: AR analytically pure;

[0059] Ethanol: chromatographically pure;

[0060]Diamine standard;

[0061] Adipic acid standard;

[0062] Nonanediamine standard;

[0063] Terephthalic acid standard;

[0064] Deionized water: laboratory grade water;

[0065] Other utensils: commonly used utensils in chemical laboratories.

[0066] Experimental steps:

[0067] a) Weigh about 0.2 g of a polyamide material sample, and decomp...

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Abstract

The invention discloses a method for identifying and quantitatively determining a polyamide material by using GC / MS. The method comprises the following steps: a) weighing a proper amount of a polyamide material sample, completely decomposing the sample into diamine hydrochloride and dibasic acid or terephthalic acid monomer by using an acid solution, filtering, and fixing the volume to form a first sample solution; b) transferring a proper amount of the first sample solution in the step a) into a constant-temperature drying oven, and evaporating at low temperature to remove redundant acid andwater to form a to-be-dissolved sample; c) re-dissolving the to-be-dissolved sample in the step b) by using a proper solvent to form a second sample solution for measurement; and d) carrying out qualitative and quantitative determination on the second sample solution by adopting a 30 m*0.25 mm*0.25 [mu]m weak-polarity chromatographic column through GC / MS. The method is simple to operate, good in repeatability and low in cost, and is completely suitable for identification and quantitative determination of polyamide materials.

Description

technical field [0001] The invention relates to a method for identification and quantitative determination of polyamide materials, in particular to a method for identification and quantitative determination of polyamide materials using GC / MS. Background technique [0002] As a class of engineering plastics with excellent performance, polyamide materials are widely used in many products in various fields. Since 1939, when the DuPont Company of the United States realized industrial production, polyamide materials have been deeply researched and developed by well-known manufacturers at home and abroad due to their good comprehensive properties, and the market has also grown extensively and rapidly. It includes a variety of varieties such as: PA6 , PA66, PA11, PA12, PA46, PA610, PA612, PAl010, etc., as well as semi-aromatic polyamides PA6T, PA9T, PA10T, etc. developed in recent years, but there are not many methods for the analysis and determination of polyamide materials. And ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/12
CPCG01N30/88G01N30/06G01N30/12G01N2030/885G01N2030/067G01N2030/126
Inventor 吴立国刘江洋
Owner 广东美塑塑料科技有限公司