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Detection method for detecting isophorone diisocyanate by using gas chromatography-mass spectrometer

A technology of isophorone diisocyanate and GC-MS, which is applied in the field of analysis, can solve the problems of undetected detection of IPDI, etc., and achieve the effect of high accuracy and good stability

Active Publication Date: 2015-02-04
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] After consulting the relevant literature and patents at home and abroad, no report on the detection of IPDI by gas chromatography or gas chromatography-mass chromatography was found.

Method used

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  • Detection method for detecting isophorone diisocyanate by using gas chromatography-mass spectrometer
  • Detection method for detecting isophorone diisocyanate by using gas chromatography-mass spectrometer
  • Detection method for detecting isophorone diisocyanate by using gas chromatography-mass spectrometer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] There is an existing batch of isophorone diisocyanate (IPDI) cargo, the quantity is 100 kg, and the effective content of IPDI in this batch of cargo needs to be tested.

[0029] The chromatographic conditions used: the chromatographic column is HP-5MS5%PhenylMethylSilox capillary column; the column temperature is 150°C for 2min, and the temperature is raised to 200°C at 5°C / min for 10min; helium is used as the carrier gas, and the carrier gas pressure is 91.92kMPa , the gas flow rate is 0.8ml / min; the gasification chamber temperature is 260°C; the split ratio is 30:1;

[0030] The mass spectrometry conditions used: ion source is EI ion source; ionization voltage is 70eV, ion source temperature is 230°C; quadrupole temperature is 150°C; transfer line temperature is 280°C.

[0031] Specific steps include:

[0032] (1) Configure IPDI standard solution

[0033] Accurately weigh 10.2mg of IPDI standard in a 100mL volumetric flask, and dilute to the mark with acetone to mak...

Embodiment 2

[0048] There is an existing batch of isophorone diisocyanate (IPDI) cargo, the quantity is 200 kg, and the effective content of IPDI in this batch of cargo needs to be tested.

[0049] The chromatographic conditions used: the chromatographic column is HP-5MS5%PhenylMethylSilox capillary column; the column temperature is 150°C for 2min, and the temperature is raised to 200°C at 5°C / min for 10min; helium is used as the carrier gas, and the carrier gas pressure is 91.92kMPa , the gas flow rate is 1.0ml / min; the gasification chamber temperature is 260°C; the split ratio is 30:1;

[0050] The mass spectrometry conditions used: ion source is EI ion source; ionization voltage is 70eV, ion source temperature is 230°C; quadrupole temperature is 150°C; transfer line temperature is 280°C.

[0051] A kind of method that utilizes gas spectrometer to detect isophorone diisocyanate (IPDI), concrete steps comprise:

[0052] (1) Configure IPDI standard solution

[0053] With embodiment 1;

...

Embodiment 3

[0068] There is an existing batch of isophorone diisocyanate (IPDI) cargo, the quantity is 500 kg, and the effective content of IPDI in this batch of cargo needs to be tested.

[0069] The chromatographic conditions used: the chromatographic column is HP-5MS5%PhenylMethylSilox capillary column; the column temperature is 150°C for 2min, and the temperature is raised to 200°C at 5°C / min for 10min; helium is used as the carrier gas, and the carrier gas pressure is 91.92kMPa , the gas flow rate is 1.5ml / min; the gasification chamber temperature is 260°C; the split ratio is 30:1;

[0070] The mass spectrometry conditions used: ion source is EI ion source; ionization voltage is 70eV; ion source temperature is 230°C; quadrupole temperature is 150°C; transfer line temperature is 280°C.

[0071] A kind of method that utilizes gas spectrometer to detect isophorone diisocyanate (IPDI), concrete steps comprise:

[0072] (1) Configure IPDI standard solution

[0073] With embodiment 1;

...

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Abstract

The invention discloses a detection method for detecting isophorone diisocyanate by using a gas chromatography-mass spectrometer. The detection method is characterized in that the gas chromatography-mass spectrometer is used for detection, an external standard method is used for analysis, an adopted chromatographic column is an HP-5MS%PhenylMethylSilox capillary chromatographic column (30m*0.25), the column temperature is 150 DEG C, the 150 DEG C temperature is maintained for 2 minutes, the temperature rises to 200 DEG C at a speed of 5 DEG C / min, and the 200 DEG C temperature is maintained for 10 minutes; nitrogen is used as a carrier gas, and the flow velocity of the carrier gas is 0.8-1.5mL / min; the temperature of a vaporizing chamber is 260 DEG C; the split ratio is 30:1; an EI ion source is adopted, the ionization voltage is 70 eV, and the ion source temperature is 230 DEG C; the temperature of a four-stage rod is 150 DEG C; the temperature of a transmission line is 280 DEG C; the injection volume is 1muL. The detection method can be used for tracing and detecting the IPDI (isophorone diisocyanate), has high accuracy and good stability, is time-saving and labor-saving and fills up the blank of the prior art.

Description

technical field [0001] The invention belongs to the technical field of analysis and relates to a method for detecting isophorone diisocyanate, in particular to a method for detecting isophorone diisocyanate by using a mass spectrometer. Background technique [0002] In recent years, my country's economic development has grown rapidly, and the domestic market has a large demand for polyurethane materials, which has led to a rapid growth in the demand for isophorone diisocyanate (IPDI). The chemical name of IPDI is 3-isocyanate methylene-3,5,5-trimethylcyclohexyl isocyanate, and its industrial product is a mixture of cis and trans isomers (3:1). IPDI is the most versatile aliphatic diisocyanate, compatible with almost all resins and all solvents. It has high relative molecular weight, low toxicity, good weather resistance, not easy to yellow, reasonable price and long service life. Compared with other isocyanates, it has better heat resistance. [0003] Isophorone diisocyana...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 董捷徐萍萍姚刚栾波
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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