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Preparation method of gas chromatography sample injection pad

A technology for gas chromatography and injection pad, which is applied in the field of preparation of gas chromatography injection pads, can solve the problems of increased cost, decreased air tightness, and inability to effectively reduce the loss of injection pads, and achieves reduction in loss, improved mechanical properties, Strength-enhancing effect

Active Publication Date: 2020-12-15
浙江迪特西科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The gas chromatography injection port septa prepared by the prior art fail to solve the problem of high temperature aging and degradation of the injection pad from the material point of view, resulting in the loss of the injection pad cannot be effectively reduced, and the number of times the injection pad is used Therefore, it is of great significance to develop a gas chromatography inlet septum with low loss at high temperature, no adhesion at the inlet, and good sealing performance after repeated use.

Method used

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  • Preparation method of gas chromatography sample injection pad
  • Preparation method of gas chromatography sample injection pad
  • Preparation method of gas chromatography sample injection pad

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Step 1, raw material pretreatment: 100g siloxane raw rubber, 35g hydrophobic modified white carbon black, 5g iron oxide, 0.5g iron trimethylsilanol at 130 o Mixing at C for 3h, then mixing in a mixture of 0.6g 2,4-dichlorodibenzoyl peroxide and 10g hydroxyl-terminated dimethyl silicone oil to obtain pretreated raw materials;

[0037] Step 2, vulcanization molding: add the pretreated raw materials into the injection pad mold of the flat vulcanizer, and o C, pre-vulcanized molding at 9 Mpa for 30 minutes to obtain a pre-vulcanized injection pad;

[0038] Step 3, post-vulcanization: put the pre-vulcanized sampling pad in a blast oven at 250 o C under treatment for 24h, to obtain a vulcanized sampling pad;

[0039]Step 4, plasma treatment: place the vulcanized sample pad in the plasma source to treat the surface, the frequency of the plasma source is 2.45GHZ, the output power is 300W, the vacuum chamber pressure is 110Pa, and the processing time is 30min to obtain the gas...

Embodiment 2

[0046] Step 1, raw material pretreatment: 100g siloxane raw rubber, 36.8g hydrophobically modified white carbon black, 6.3g titanium dioxide, 0.7g1,1'-bis(dimethylsilyl)ferrocene at 135.4 o Mixing at C for 2.6h, then mixed with a mixture of 0.7g tert-butyl peroxybenzoate and 10.6g hydroxy-terminated methylphenyl silicone oil, to obtain pretreated raw materials;

[0047] Step 2, vulcanization molding: add the pretreated raw materials into the injection pad mold of the flat vulcanizer, at 164 o C, pre-vulcanized molding at 10.4 Mpa for 26.7 minutes to obtain a pre-vulcanized injection pad;

[0048] Step 3, post-vulcanization: put the pre-vulcanized sampling pad in a blast oven at 245 o C under treatment for 26.4h, to obtain a vulcanized sampling pad;

[0049] Step 4, plasma treatment: place the vulcanized sampling pad in the plasma source to treat the surface, the frequency of the plasma source is 2.45GHZ, the output power is 336W, the pressure of the vacuum chamber is 117.8Pa...

Embodiment 3

[0056] Step 1, raw material pretreatment: 100g siloxane raw rubber, 38.9g hydrophobic modified white carbon black, 7.6g chromium trioxide, 0.9g trimethylsilanol iron at 139 o Mixing at C for 2h, then mixed with a mixture of 0.8g di-tert-butyl peroxide and 11.7g hydroxyl-terminated diphenyl silicone oil, to obtain pretreated raw materials;

[0057] Step 2, vulcanization molding: add the pretreated raw materials into the injection pad mold of the flat vulcanizing machine, at 170.4 o C, pre-vulcanized molding under 10.9Mpa for 25.2min to obtain a pre-vulcanized injection pad;

[0058] Step 3, post-vulcanization: put the pre-vulcanized sample pad into the blast oven, o C under treatment for 33.1h, to obtain a vulcanized sampling pad;

[0059] Step 4, plasma treatment: place the vulcanized injection pad in the plasma source to treat the surface, the frequency of the plasma source is 2.45GHZ, the output power is 368W, the pressure in the vacuum chamber is 121.4Pa, and the treatmen...

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Abstract

The invention discloses a preparation method of a gas chromatography sample injection pad. The preparation method comprises the following steps: step 1. pretreatment of raw materials: mixing siloxaneraw rubber, hydrophobic modified white carbon black, toner and a high-temperature-resistant assistant at 130-160 DEG C for 1-3h, and mixing with a mixture of a vulcanizing agent and silicone oil to obtain a pretreated raw material; step 2, vulcanization molding: adding the pretreated raw materials into a sample injection pad mold of a press vulcanizer, and carrying out prevulcanization molding at160-200 DEG C and 9-14 Mpa for 15-30 minutes to obtain a prevulcanized sample injection pad; step 3, post-vulcanization: putting the pre-vulcanized sample injection pad into a blast drying oven, and treating for 24-48h at 200-250 DEG C to obtain a vulcanized sample injection pad; and step 4, plasma treatment: the vulcanized sample injection pad is placed in a plasma source for surface treatment, the frequency of the plasma source is 2.45 GHZ, the output power of the plasma source is 300-500 W, the air pressure of a vacuum chamber is 110-140 Pa, the treatment time is 10-30 min, and the gas chromatography sample injection pad is obtained. The sample injection pad obtained by the method has lower high-temperature loss and higher strength and resilience sealing performance.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method of a gas chromatography sample pad. Background technique [0002] Gas chromatography plays an important role in the convenience of sample composition analysis, and is an indispensable analysis method in the modern chemical and material industries. As a part of gas chromatography, the gas chromatography injection pad has a significant impact on the performance of the gas chromatography. The high-quality injection port septum will not introduce impurities during the gas chromatography analysis process, so that the obtained spectrum has no background noise. The influence greatly improves the accuracy of spectrum detection. [0003] However, most gas chromatographic septa degrade at high temperature during use, and the small molecules inside will diffuse into the gas chromatograph, causing background interference in the gas chromatograph, thus requiring updated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/08C08L83/04C08K9/06C08K7/26C08K5/14C08K5/56C08K3/22C08K13/06C08K3/30
CPCC08L83/08C08K2003/2265C08K2003/2241C08K2003/2251C08K2003/3027C08L2201/08C08L2205/02C08L2201/14C08L83/04C08K9/06C08K7/26C08K5/14C08K5/56C08K3/22C08K13/06C08K3/30
Inventor 傅强韩强俞慧萍付晓苗周游
Owner 浙江迪特西科技有限公司