CN107607528A - The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance - Google Patents

The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance Download PDF

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Publication number
CN107607528A
CN107607528A CN201710705401.0A CN201710705401A CN107607528A CN 107607528 A CN107607528 A CN 107607528A CN 201710705401 A CN201710705401 A CN 201710705401A CN 107607528 A CN107607528 A CN 107607528A
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China
Prior art keywords
poisonous
optical
harmful substance
fibre needle
recognizable
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Pending
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CN201710705401.0A
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Chinese (zh)
Inventor
王华山
黄哲
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Tianjin University of Science and Technology
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Tianjin University of Science and Technology
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Priority to CN201710705401.0A priority Critical patent/CN107607528A/en
Publication of CN107607528A publication Critical patent/CN107607528A/en
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The invention provides a kind of preparation method of the optical-fibre needle of recognizable poisonous and harmful substances, its preparation process includes poisonous and harmful substance to be measured, polymer, auxiliary reagent etc. being blended, extrusion stretching is prepared into optical fiber, then poisonous and harmful substance extracted being truncated into pin front/rear be put into extraction solution, i.e. finished product.The extract of testing sample or testing sample is inserted during use, by the absorption of certain time, takes out optical-fibre needle, judges that poisonous and harmful substance whether there is and corresponding content by the change of its optical characteristics.The invention has the characteristics of easy to use, easy directly piercing testing sample, high specificity.

Description

The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance
Technical field
The invention belongs to technical field of analysis and detection, and in particular to a kind of optical-fibre needle of recognizable poisonous and harmful substance Preparation method.
Background technology
In recent years, it is the environmental pollution that triggers due to the high speed development of industry, a large amount of applying pesticides chemical fertilizer of agricultural production, illegal The food-safety problem being on the rise that additive etc. is brought, in field of food safety, the quick hair of new analysis and detection technology Exhibition is particularly important.Instrument analytical method based on principles such as chromatogram, spectrum is normal in venomous injurant quality detection in food One of method, pre-treatment of this kind of method generally to sample requires very strict, and needs to give testing staff training, Take time and effort, frequently can lead to market monitorings hysteresis, a large amount of underproof agricultural product, food flow to market.
Based on above reason, as country is in the increasing of Food Quality and Safety field relation technological researching supporting dynamics, In good time, accurate, convenient, high specificity detection method has become food safety detection, poisonous and harmful substance identification process Fresh target and new demand.
The content of the invention
It is in view of the deficienciess of the prior art, recognizable poisonous the technical problem to be solved by the invention is to provide one kind The preparation method of the optical-fibre needle of harmful substance, two innovative thinkings of the invention, first, detection articles for use are designed to needle-like, and It is combined with the processing and forming of corresponding high polymer material, knows second, being fixed based on dye indicator on transparent article with optical property Other detection mode, the inventive method have the characteristics of easy to use, high specificity.Food security is concerning common people's health and society The significant problem that can stablize, the present invention and a thing for being beneficial to people's health.
The present invention adopts the technical scheme that, a kind of preparation method of the optical-fibre needle of recognizable poisonous and harmful substance, including The following steps:
(1) auxiliary reagent prepares:According to identification object feature, auxiliary reagent includes monomer indicator, processing aid.
(2) optical fiber is molded:After pin material, auxiliary reagent, poisonous and harmful substance to be measured are well mixed, co-extrusion rear haulage is melted Stretching obtains optical fiber;
(3) noxious material is extracted:Optical fiber made from (2) is had poisonous being truncated into front/rear be put into extraction solution of pin Evil extracting substances come out;Obtain surveying the optical-fibre needle of poisonous and harmful substance.
(4) demarcate:Part finished product made from (3) is inserted to the extract of standard sample or standard testing sample to be measured, warp The absorption of certain time is crossed, takes out optical-fibre needle;Poisonous and harmful substance is demarcated with the presence or absence of/or phase by the change of its optical characteristics The content answered.
Wherein, step (1) described indicator is dithizone, p-aminobenzene sulfonic acid, phenol reagent, ferrocyanide, thio second One or more in acid amides, rhodamine.The processing aid is surfactant, initiator, coupling agent, crosslinking agent, anti- One or more in oxygen agent.
Step (2) the pin material includes polymethacrylates, makrolon, polystyrene, polyketone, polyether-ether-ketone, poly- At least one of acid imide, glass.The poisonous and harmful substance includes agricultural chemicals, heavy metal, nitrite, formaldehyde, titanium dioxide At least one of sulphur, benzene, hydrogen peroxide
Wherein, step (1) (2) described mixed process includes one kind in melt blending, solution blending, monomer in situ polymerization It is or several.
The Cleaning Principle of optical-fibre needle of the present invention is:It is poisonous and harmful after testing sample is combined with indicator by pre-treatment Material is reacted with indicator, produces color change, chemical information is changed into optical information, qualitative or fixed to carry out with this Amount detection.
The advantages of the present invention:
1st, the optical-fibre needle for preparing of the present invention is solid-state, can according to using arbitrarily blocking, compared with traditional detection analysis method, Using more convenient, and high specificity, service efficiency is high, and Detection results are obvious.
2nd, the invention provides a kind of optical-fibre needle of recognizable poisonous and harmful substance, food hygiene peace can be efficiently applied to Full detection field.
Embodiment
Embodiment is used for the further explanation to the present invention below, but is not limited to the scope of the present invention.
Embodiment 1
(1) prepared by auxiliary reagent:0.85g phenol is shown into agent, 0.65g glycerol stearates monoesters, 0.1g antioxidant 1010s, 0.4g Coupling agent KH570 is mixed, and puts into and 3min is ground in pulverizer, it is ensured that and it is well mixed, obtain auxiliary agent.
(2) optical fiber is molded:75g polymethylmethacrylapellets pellets auxiliary agent obtained with (1) and 6g is to be measured poisonous containing formaldehyde Put into after harmful substance is well mixed in high-speed mixer, 50 DEG C, incorporation time 25min of mixing temperature, extruded on extruder, Traction stretching obtains optical fiber;
(3) noxious material is extracted:Optical fiber made from (2) is extracted formaldehyde being truncated into being put into before pin in toluene or n-hexane Take out, obtain surveying the optical-fibre needle of poisonous and harmful substance.
Or formaldehyde is extracted to obtained fiber cut into being put into toluene or n-hexane after pin, obtain surveying The optical-fibre needle of poisonous and harmful substance.
(4) demarcate:Part finished product made from (3) is inserted to the extract of standard sample or standard testing sample to be measured, warp The absorption of certain time is crossed, optical-fibre needle is taken out after 6min, there is faint yellow generation, by the optical-fibre needle after discoloration and commercially available formaldehyde standard Colorimetric card color contrast, select the concentration of formaldehyde scope of color close calorific power, as testing sample.
Embodiment 2
(1) prepared by auxiliary reagent:1.4g p-aminobenzene sulfonic acid, 0.8g odium stearate, 0.1g antioxidant 1010s, 0.3g are handed over Join agent DCP mixing, and put into and 5min is ground in pulverizer, it is ensured that it is well mixed, obtain auxiliary agent.
(2) optical fiber is molded:70g polycarbonate pellets auxiliary agent obtained with (1) and 5g is to be measured poisonous and harmful containing nitrite Material mixing is uniformly put into high-speed mixer afterwards, 60 DEG C, incorporation time 30min of mixing temperature, is extruded, is drawn on extruder Stretching obtains optical fiber;
(3) noxious material is extracted:Optical fiber made from (2) is being truncated into being put into before pin in water or diluted alkaline extraction solution by Asia Nitrate extracts, and obtains surveying the optical-fibre needle of poisonous and harmful substance.
Or nitrite is extracted to obtained fiber cut into being put into after pin in water or diluted alkaline extraction solution, Obtain surveying the optical-fibre needle of poisonous and harmful substance.
(4) demarcate:Part finished product made from (3) is inserted to the extract of standard sample or standard testing sample to be measured, warp The absorption of certain time is crossed, optical-fibre needle is taken out after 15min, has light red brown to produce, by the optical-fibre needle after discoloration and commercially available nitrous Hydrochlorate standard color comparison card color contrast, select the nitrite concentration scope of color close calorific power, as testing sample.
Embodiment 3
(1) prepared by auxiliary reagent:By 0.75g rhodamine Bs and 0.5ml hydrazine hydrates under nitrogen protection, in absolute ethyl alcohol body 12h is stirred at reflux in system, after removing solvent, organic phase is extracted with dichloromethane and water, dries, is filtrated to get auxiliary agent.
(2) optical fiber is molded:Auxiliary agent, 0.5g neopelexes, 0.15g is made in 80g polystyrene pellets and (1) Put into after antioxidant 1010,0.4g coupling agent KH550 and 10g determinand containing Cu are well mixed in high-speed mixer, mixing temperature 60 DEG C, incorporation time 40min, extruded on extruder, traction stretching obtains optical fiber;
(3) noxious material is extracted:Optical fiber made from (2) is extracted Cu being truncated into being put into diphenyl-ketoxime before pin Come, obtain surveying the optical-fibre needle of poisonous and harmful substance;
Or Cu is extracted to obtained fiber cut into being put into diphenyl-ketoxime after pin, obtain surveying poisonous The optical-fibre needle of harmful substance.
(4) demarcate:Part finished product made from (3) is inserted to the extract of standard sample or standard testing sample to be measured, warp The absorption of certain time is crossed, optical-fibre needle is taken out after 10min, there is pink generation, Cu presence causes the network with indicator molecules Cooperation generates color change with intramolecule open loop is caused.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art For, on the premise of inventive concept is not departed from, various modifications and improvements can be made, these belong to the protection of the present invention Scope.

Claims (7)

  1. A kind of 1. preparation method of the optical-fibre needle of recognizable poisonous and harmful substance, it is characterised in that:Comprise the following steps:
    (1) auxiliary reagent prepares:According to identification object feature, auxiliary reagent includes monomer indicator, processing aid;
    (2) optical fiber is molded:After pin material, auxiliary reagent, poisonous and harmful substance to be measured are well mixed, the rear haulage stretching of melting co-extrusion Obtain optical fiber;
    (3) noxious material is extracted:By optical fiber made from (2), pin is front/rear to be put into venomous injurant in extraction solution being truncated into Matter extracts, and obtains surveying the optical-fibre needle of poisonous and harmful substance.
  2. A kind of 2. preparation method of the optical-fibre needle of recognizable poisonous and harmful substance, it is characterised in that:Comprise the following steps:
    (1) auxiliary reagent prepares:According to identification object feature, auxiliary reagent includes monomer indicator, processing aid;
    (2) optical fiber is molded:After pin material, auxiliary reagent are well mixed, melting co-extrusion rear haulage stretches to obtain optical-fibre needle.
  3. 3. the preparation method of the optical-fibre needle of recognizable poisonous and harmful substance according to claim 1 or 2, it is characterised in that: The auxiliary reagent is one in dithizone, p-aminobenzene sulfonic acid, phenol reagent, ferrocyanide, thioacetamide, rhodamine Kind is a variety of.
  4. 4. the preparation method of the optical-fibre needle of recognizable poisonous and harmful substance according to claim 1 or 2, it is characterised in that: The processing aid is the one or more in surfactant, initiator, coupling agent, crosslinking agent, antioxidant.
  5. 5. the preparation method of the optical-fibre needle of recognizable poisonous and harmful substance according to claim 1 or 2, it is characterised in that: The pin material be polymethacrylates, makrolon, polystyrene, polyketone, polyether-ether-ketone, polyimides, in glass extremely Few one kind.
  6. 6. the preparation method of the optical-fibre needle of recognizable poisonous and harmful substance according to claim 1 or 2, it is characterised in that: The poisonous and harmful substance is at least one of agricultural chemicals, heavy metal, nitrite, formaldehyde, sulfur dioxide, benzene, hydrogen peroxide.
  7. 7. the preparation method of the optical-fibre needle of recognizable poisonous and harmful substance according to claim 1, it is characterised in that described It is mixed into melt blending, solution blending, monomer in situ polymerization.
CN201710705401.0A 2017-08-17 2017-08-17 The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance Pending CN107607528A (en)

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CN201710705401.0A CN107607528A (en) 2017-08-17 2017-08-17 The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance

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Application Number Priority Date Filing Date Title
CN201710705401.0A CN107607528A (en) 2017-08-17 2017-08-17 The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance

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CN107607528A true CN107607528A (en) 2018-01-19

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1488784A (en) * 2003-08-13 2004-04-14 东华大学 Long-persistence luminous composite fiber and preparing method thereof
CN101359073A (en) * 2008-09-27 2009-02-04 沈志伟 Reinforced core and optical cable using the reinforced core

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1488784A (en) * 2003-08-13 2004-04-14 东华大学 Long-persistence luminous composite fiber and preparing method thereof
CN101359073A (en) * 2008-09-27 2009-02-04 沈志伟 Reinforced core and optical cable using the reinforced core

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