CN106959350A - A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument - Google Patents
A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument Download PDFInfo
- Publication number
- CN106959350A CN106959350A CN201710213660.1A CN201710213660A CN106959350A CN 106959350 A CN106959350 A CN 106959350A CN 201710213660 A CN201710213660 A CN 201710213660A CN 106959350 A CN106959350 A CN 106959350A
- Authority
- CN
- China
- Prior art keywords
- sample
- base salt
- detection
- automated synthesis
- cyanic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument, including flow path system, specimen inspection system, embedded Webserver.The flow path system includes microelectronics multiposition valve, precise injection pump, direct current peristaltic pump, pipeline；Flow path system connects sample, detection reagent, distilled water, sample conversion reaction pond respectively.The specimen inspection system includes LED light source, sample detection room, photodiode, the LED light source is through the first collimated emitting parallel light, through sample detection room, then by the second lens focus photovoltage output is directly translated into the optical window of photodiode.The embedded Webserver includes power module, and embedded Webserver sends control command, control flow path system, specimen inspection system by serial ports, while obtaining the data of specimen inspection system output by serial ports and dealing with analysis.The present invention can realize that full-automatic, quick detection is analyzed to the base salt sample solution of artificial simple pretreated normal concentration scope.
Description
Technical field
The invention belongs to metallurgy industry QPQ salt bath compound base amount method technical fields, specifically a kind of QPQ technologies base salt cyanogen
Acid group content fully-automated synthesis analytical instrument, analysis reference is provided for the quality control of QPQ technical matters.
Background technology
QPQ (abbreviation of " Quench-Polish-Quench ") is a kind of salt bath composite articles process for treating surface.It is former
Quenching-polishing-quenching is meant, but above-mentioned " quenching " is not conventional quenching concept known to us, and refer to metal at two kinds
Make Combined Processing in high-temperature molten salt bath of different nature, so that carbon, nitrogen penetrate into metal surface simultaneously, formed by nitride
The compound layer diffuseed to form with oxide, makes metal surface be strengthened modification, while can increase substantially metal watch again
The wearability in face, corrosion stability, this metal surface enhanced modification technology realize nitriding process and oxidation operation (carbo-nitriding)
It is compound, nitride and oxide it is compound, wearability and corrosion stability are compound, heat treatment technics and aseptic technic it is compound.Should
Technology obtains substantial amounts of popularization and application at home at present, especially in automobile, motorcycle, axis products, electronic component, frame, machine
Bed, electric switch, using effect is protruded very much on tool and mould.It has wearability, corrosion resistance and the endurance of enhancing workpiece
Property, technical process low cost, the technical advantage of low-carbon environment-friendly.
QPQ technical qualitys control be related to carbo-nitriding temperature, the carbo-nitriding time, base salt cyanic acid radical content control etc. because
Element.The detection of cyanate content (with cyanate radical C NO- Molecular weights) wherein in base salt component is the control of QPQ technical qualitys
Important indicator, cyanic acid radical content should be generally controlled in the range of the 32%-38% of mass fraction, when cyanate radical content by
Mass fraction increases to 38% for 32%, under conditions of same nitriding temperature and nitridation time (570 in such as titanium alloy smelting furnace
DEG C, 2.5h nitridation under conditions of, using 45 steel samples as subjects), with nitridation salt bath in cyanic acid radical content rise, carbon nitrogen
Permeation compound layer depth straight line increase, because the rise of CNO-content so that the concentration rise (cyanic acid of atomic state nitrogen
Root decomposes generation nitrogen-atoms at high temperature), accelerate the formation speed of compound layer.Experiment is found, when base salt cyanic acid in salt bath
When radical content is less than the 32% of mass fraction, element permeating speed can significantly decline, under similarity condition, the depth of compound layer
It can greatly reduce；When cyanate content is higher than the 38% of mass fraction in salt bath, then the oxidisability enhancing of salt bath, the change of formation
Compound layer can bring serious loose.Therefore, the mass fraction of general cyanic acid radical content should control the normal model in 32%-38%
In enclosing, such as it is higher than 40%, then can raises salt temperature, cyanate radical automatic classifying is reduced its content to proper range, if being less than
32%, then the content of adjustment salt rise cyanate radical must be added in proportion to proper range.Therefore, it is excessively program control from QPQ technical qualitys
The angle analysis of system needs quick and precisely to detect the content of cyanate radical in base salt component.However, present analysis instrument market does not have but
There is the automatical analysis instrument that can detect cyanic acid radical content, current most of QPQ technological development or application industry, such as east wind vapour
Car hydraulic power Co., Ltd, Chengdu Tool Research Institute Co., Ltd. etc. are equipped with dedicated technician, manual sampling, by numerous
Trivial and complicated manual laboratory's analysis method (formaldehyde nitriding) detects the content of base salt cyanate radical, but manual titration tests
Detecting step is more, poor repeatability, may introduce larger human error, and the quality control for being difficult to QPQ technologies provides accurate
Technical support referred to analysis, this exactly China current workpiece surface carbo-nitriding QPQ Quench-Polish-Quench technology technology faces
One technical barrier.
Simultaneously as workpiece surface QPQ technical finesses carry out in salt in are melted for high-temperature titanium alloy smelting furnace, it is difficult to base
Cyanic acid radical content in salt component realizes on-line monitoring analysis, and only preferably a manual sampling is simultaneously cooled to room temperature, and then accurate weighing is again
Plus distilled water constant volume is into carrying out content detection after the sample solution of regulation concentration range.Therefore, in order to meet QPQ technical quality mistakes
The technical requirements that process control is analyzed base salt component quick detection, are adapted to exploitation fully-automated synthesis instrument dense to the regulation prepared
The base salt sample solution for spending scope carries out quick directly detection and analysis.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analysis
Instrument, can realize that full-automatic, quick detection is analyzed to the base salt sample solution of artificial pretreated normal concentration scope.
The technical scheme that the present invention takes is：
A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument, including flow path system, sample detection system
System, embedded Webserver.
The flow path system includes microelectronics multiposition valve, precise injection pump, direct current peristaltic pump, pipeline；Flow path system is distinguished
Connect sample, detection reagent, distilled water, sample conversion reaction pond, the microelectronics multiposition valve, precise injection pump, direct current
Peristaltic pump connects embedded Webserver.
The specimen inspection system includes LED light source, sample detection room, photodiode, and the LED light source is saturating through first
Mirror collimates emitting parallel light, through sample detection room, then enters the optical window of photodiode by the second lens focus, directly turns
It is changed into photovoltage output.
The embedded Webserver includes power module, and embedded Webserver sends control command by serial ports, controls
Flow path system processed, specimen inspection system, while obtaining the data of specimen inspection system output by serial ports and dealing with analysis.
The functions such as concise sampling, cleaning, the waste discharge of the flow path system, microelectronics multidigit is driven by embedded Webserver
Valve, precise injection pump and direct current peristaltic pump are completed, and produced waste liquid enters waste liquid pool.
The sample detection room is intersecting for flow path system and specimen inspection system, i.e. stream and light path is intersected.
The microelectronics multiposition valve has multi-channel flow passage handoff functionality, and its common port connects liquid storage ring one by PEEK pipes
End, the liquid storage ring other end connects a flow path channel of precise injection pump, another changeable stream of precise injection pump
Passage connects distilled water pond by PEEK pipes.
The sample conversion reaction pond includes stainless steel sealed taper shaped reaction room, constant temperature water bath pond, microelectronics multiposition valve
Valve position 11# connects sample detection room by PEEK pipes.The valve position 9# of the microelectronics multiposition valve connects sample by PEEK pipes and turned
Change the stainless steel sealed taper shaped reaction room of reaction tank.The valve position 10# of the microelectronics multiposition valve connects sample by PEEK pipes and turned
Change the constant temperature water bath pond of reaction tank.The valve position 8# connection waste liquid pools of the microelectronics multiposition valve.
Constant temperature water bath pond material be stainless steel, its bottom integrated heating pipe, for the heating to sample conversion reaction,
When reaction system is freezed, heating tube power-off.
The sample detection room includes aluminium cell body, the cuvette being mounted in aluminium cell body, and cuvette is quartz
Heating rod is installed in glass material, the aluminium cell body bottom, is conducted heat by temperature control and air, realizes and is reacted in contrastive colours cup
The thermostatic control of solution.
Photoelectric Detection module is equipped with the aluminium cell body：Light emitting diode and photodiode, the light-emitting diodes
The example reaction solution in detection light beam tranmittance color cup that pipe is sent, into photodiode, through opto-electronic conversion, by absorbing
Spectrum analysis detects sample concentration.
The embedded Webserver includes power module, embedded processing module, peripheral control circuits, data acquisition electricity
Road；The embedded processing module connects peripheral control circuits, and peripheral control circuits are used to realize light source drive control, stream control
System, temperature control.The embedded processing module connects data acquisition circuit, and data acquisition circuit is connected by circuit for signal conditioning
Connect photodiode.
The embedded processing module is connected with man-machine interactive system by serial ports, man-machine interactive system include memory,
Touch-control LCD display and gprs system, gprs system are connected by being wirelessly transferred with host computer.
The embedded processing module core is SAMSUNGS3C6410 microprocessors, using linux kernel technology.
A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analysis method, cyanate content detection is using inspection indirectly
Survey method, first passes through chemical method and cyanate radical CNO- is changed into ammonium root NH4+, as shown in (1) formula, then establishing criteria GB7481-
1987：The measure salicylic acid AAS of water quality ammonium, by the measure to ammonium ion, detection characteristic wavelength is 697nm, indirectly
Realize the detection to cyanate content.
OCN-+2H++H2O=NH4 ++CO2↑ (1)。
A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument of the present invention, technical advantage is as follows：
1st, the present invention can replace the artificial experimental analysis of current QPQ technologies base salt cyanate radical content detection completely, repeat
Property it is good, the degree of accuracy is high, and important technology can be provided for workpiece surface QPQ technical finesse quality controls and is supported with analyzing reference.
2nd, the present invention is based on characteristic wavelength LED light source needed for corresponding detection module and photodiode single spectrum detection skill
Art, replaces the formol titration of industry routine to detect the content of cyanate radical, accuracy of detection is high, detection cycle using spectrum analysis
It is short.
3rd, the detection reagent of the invention used is anti-interference by force, can be used at normal temperatures, improves the essence of spectral detection
Exactness and repeatability.
4th, the present invention improves spectrum inspection to the accurate thermostatic control technology of example reaction system sampling and mixing control technology
The accuracy and stability of survey.
Brief description of the drawings
Fig. 1 is the detection method flow chart of the present invention.
Fig. 2 is the stream schematic diagram of the detecting instrument of the present invention.
Fig. 3 is the temperature control system schematic diagram of the present invention.
Fig. 4 is the measurement and control system schematic diagram of the present invention.
Fig. 5 is the instrumental calibration and detection principle diagram of the present invention.
Fig. 6 is the workflow diagram of the present invention.
Embodiment
It is as follows to this embodiment with reference to accompanying drawing：
As shown in figure 1, a kind of QPQ technologies base salt component fully-automated synthesis analytical instrument application flow, is tested the sampling of base salt
Be cooled to after room temperature, through accurate weighing, pretreatment and constant volume into regulation concentration range sample solution after, that is, send fully-automated synthesis
Analytical instrument detects the content of cyanate radical.
Cyanate radical detection uses Indirect Detecting Method, first passes through chemical method and cyanate radical (CNO-) is changed into ammonium root (NH4
+), then establishing criteria GB7481-1987 (the measure salicylic acid AAS of water quality ammonium) passes through (detection of measure to ammonium ion
Characteristic wavelength is 697nm) detection of the realization to cyanate content indirectly.
As shown in Fig. 2 a kind of QPQ technologies base salt component fully-automated synthesis analytical instrument, the flow path system includes multidigit
Valve 1, syringe pump 2, direct current peristaltic pump, pipeline.
Its flow path system principle is expressed as follows：The multiposition valve 1 (integrated control module) and the integrated control mould of syringe pump 2
Block) constitute the handoff functionality with many flow path channels；With the accurate sequential injection flow path system for pumping function of reagent and sample,
The multiposition valve 1 has multi-channel flow passage handoff functionality, and its common port 4 connects the one end of liquid storage ring 5, the liquid storage by PEEK pipes
The other end of ring 5 connects a flow path channel of syringe pump 2, and another changeable flow path channel of syringe pump 2 is connect by PEEK pipes
Logical distilled water pond 6.The valve position 11# of multiposition valve 1 connects sample detection room 7 by PEEK pipes.The valve position 9# of multiposition valve 1 passes through
The stainless steel sealed taper shaped reaction room 9 in PEEK pipes connection sample conversion reaction pond 8.The valve position 10# of the multiposition valve 1 passes through PEEK
The constant temperature water bath pond 10 in pipe connection sample conversion reaction pond 8.Remaining valve bit stream road handoff functionality of multiposition valve 1 is also as shown in Figure 2.
As shown in Fig. 2 the flow path system has the accurate extraction of stream switching, sample and reagent；It is automatic with stream
Cleaning function.It is specified as：Control the rotor 11 ' of multiposition valve 1, its internal rotary pipeline, can make common port 4 with
Connect sample solution, detection reagent, distilled water, freezing liquid, air, waste liquid pool 12, sample conversion reaction pond 8, sample detection room 7
Valve position stream conducting so that realize stream switch.
When stream works, control syringe pump 2 and multiposition valve 1 try the sample solution of certain volume with corresponding dilute sulfuric acid
Agent and sodium hydroxide reagent are pumped into liquid storage ring 5 successively, and then the rotor of multiposition valve 1 goes to valve position 9#, and syringe pump 2 is counter to be pushed away, you can
Sample solution and reaction reagent push-in sample conversion reaction pond 8, reaction inside makes cyanate radical be converted into ammonium root.Then control is noted
Penetrate pump 2 and multiposition valve 1, the preprocessing solution of certain volume in sample conversion reaction pond 8 with corresponding bigcatkin willow acid reagent 1. and
2. bigcatkin willow acid reagent is pumped into liquid storage ring 5 successively, and then the rotor of multiposition valve 1 goes to valve position 11#, and syringe pump 2 is counter to be pushed away, you can pre-
Processing solution and reaction reagent push-in sample detection room 7, complete chromogenic reaction and sample spectra detection inside.
During cleaning, syringe pump 2 and multiposition valve 1 are first controlled, sample conversion reaction pond 8 or the waste liquid of sample detection room 7 are extracted into
In liquid storage ring 5, then the rotor of multiposition valve 1 goes to valve position 8#, shifts waste liquid pool 12 onto waste liquid is counter, then controls stream to extract and distills
Water rinses sample conversion reaction pond 8 or sample detection room 7, and waste liquid is similarly transported to waste liquid pool 12.
As shown in Fig. 2 the sample conversion reaction pond 8 of the flow path system is permanent by stainless steel sealed taper shaped reaction room 9, water-bath
Warm pond 10 is constituted, and the material of constant temperature water bath pond 10 is stainless steel, and its bottom integrated heating pipe 11 is anti-to sample conversion to realize
The heating answered.When reaction system is freezed, heating tube 11 is powered off, first by hot water in the drained constant temperature water bath pond 10 of stream principle, then
Control stream to extract the freezing liquid of certain volume again, circulate pump drainage to reduce reaction system in stainless steel sealed taper shaped reaction room 9
Temperature.
Stainless steel sealed taper shaped reaction room 9, the reative cell uses conical lower portion, is easy to the 9# valves position with multiposition valve 1 to connect
The capillary stainless steel tube connect completely attaches to the bottom of taper reative cell 9, will pass through the effect of syringe pump 2 and multiposition valve 1, realizes anti-
The complete transfer of solution is answered, that is, is completely transferred to example reaction sensing chamber 7.
The specimen inspection system includes LED light source, sample detection room 7, photodiode, and the LED light source is through first
Lens 13 collimate emitting parallel light, through sample detection room 7, then the light for entering photodiode is focused on by the second lens 14
Window, is directly translated into photovoltage output.
As shown in Fig. 2 the sample detection room 7 is fixed in aluminium cell body 20 by aluminium cell body 20 and by mechanical erection
Cuvette 19 is constituted, and cuvette 19 is quartz glass material, and heating rod 21 is installed in the bottom of aluminium cell body 20, by temperature control and
Air conducts heat, and realizes the thermostatic control of reaction solution in contrastive colours cup 19.The exterior bottom of sample detection room 7 is external straight by pipeline
Peristaltic pump 30 is flowed, waste reaction solution is discharged to waste liquid pool 12.
Photoelectric Detection module is equipped with the aluminium cell body 20：Light emitting diode 22 and photodiode 23, the hair
The detection light beam 24 that optical diode 22 is sent is through the example reaction solution in cuvette 19, into photodiode 23, through light
Electricity conversion, ammonium root concentration in sample solution is detected by absorption spectroanalysis.
As shown in Figure 3：Cryocooler Temperature Closed Loop Control System is by single-chip microcomputer, K-type thermocouple temperature sensor, relay and heating tube
Constitute.The single-chip microcomputer can by key-press input set temperature value and pid control parameter, charactron can show set parameter and by
Control object real-time temperature values.The controlled device real-time temperature values are gathered in real time by K-type thermocouple temperature sensor, and single-chip microcomputer is obtained
Obtain after real-time temperature values, by pid algorithm output control signal, reached by the working condition of the relay driving heating tube
Temperature control purpose.
As shown in figure 4, the embedded Webserver includes measuring circuit module, control circuit module, embedded processing
Man-machine interactive system, man-machine interactive system are connected with by serial ports in module 15 and power module 16, embedded processing module 15
Including memory 29, touch-control LCD display 25 and gprs system 26, gprs system 26 is connected by being wirelessly transferred with host computer 27
Connect.The data acquisition circuit of measuring circuit module is connected in embedded processing module 15 by serial ports, sample Photoelectric Detection is obtained
Information.Control circuit module is connected by serial ports in embedded processing module 15, by peripheral control circuits 17, stream control is sent
The control commands such as system, temperature control, light source drive control.
The flush bonding module core is SAMSUNGS3C6410 microprocessors, using linux kernel technology.
The power module 16 is embedded Webserver, peripheral control circuits 17 are powered.
The measuring circuit module includes light source LED LED (centre wavelength 697nm) drive circuit, Signal Regulation
Circuit 28 and data acquisition circuit 18.Light source LED LED drive circuit using constant-current source drive, electric current it is constant
20mA, has control port to control emitting led switch.Photoelectric conversion signal uses accurate discharge circuit by the micro- of photodiode
Weak current signal is converted to voltage signal, then amplifies by two stage amplifer changed voltage signal, and multiplication factor can pass through
Accurate slide rheostat debugging, it is ensured that detection signal prevents that saturation from amplifying in linear scope, then will by 13 A/D converters
Analog signal is converted to data signal and uploads to embedded processing module 15 by serial ports.
As shown in figure 5, the demarcation of instrument of the present invention and Cleaning Principle are specified as：
(1) demarcate：
The ammonium chloride standard sample solution of respective concentration gradient is prepared with distilled water, with standard sample solution replacement Fig. 2
Tested salt sample Solutions Solution, control syringe pump 2 and multiposition valve 1, standard sample solution and the corresponding bigcatkin willow of certain volume
2. 1. acid reagent is pumped into liquid storage ring 5 successively with bigcatkin willow acid reagent, and then the rotor of multiposition valve 1 goes to valve position 11#, syringe pump 2
It is counter to push away, standard sample solution and reaction reagent are pushed into sample detection room 7, chromogenic reaction is completed in sample detection room 7 and is examined
The absorbance A of reaction system is surveyed, with the concentration C abscissa of standard liquid, using corresponding absorbance A as ordinate, minimum is utilized
Two, which multiply principle, fits standard working curve, and standard working curve is cured into embedded Webserver.
(2) detect：
For tested base salt sample solution, first complete after sample conversion, sample is converted anti-in sample conversion reaction pond 8
The preprocessing solution of certain volume in pond 8 is answered 1. 2. to be pumped into liquid storage ring 5 successively with bigcatkin willow acid reagent with corresponding bigcatkin willow acid reagent
Interior, then the rotor of multiposition valve 1 goes to valve position 11#, and syringe pump 2 is counter to be pushed away, and preprocessing solution and reaction reagent are pushed into sample detection
Room 7, completes chromogenic reaction and detects absorbance A inside, and absorbance A, which is finally substituted into standard working curve, can calculate sample
The concentration of middle ammonium root, is thus calculating the content of cyanate in sample indirectly.
As shown in fig. 6, the present invention workflow for instrument initialization, sample conversion, blank detection, sample detection, consolidate
Body salt sample cyanate radical five steps of content analysis.
The instrument initialization includes the steps such as instrument self checking, stream cleaning, light stability；
The sample conversion is that the cyanate radical in sample solution is changed into ammonium root, is easy to subsequent detection；
The blank measure is measurement reagent blank value, i.e. measurement and the isometric distilled water of sample solution and certain body
Product colour reagent (bigcatkin willow acid reagent 1., bigcatkin willow acid reagent 2.) mix after absorbance, the purpose is to eliminate chromogenic reaction mistake
Measure reagent interference；
The sample detection is sample solution and certain volume colour reagent (bigcatkin willow after measurement certain volume pretreatment conversion
Acid reagent 1., bigcatkin willow acid reagent 2.) absorbance after chromogenic reaction, and deduct blank value, then to substitute into standard of instruments work bent
Line, you can calculate ammonium root concentration in tested pretreatment sample solution.
Solid Slat cyanate radical content analysis, refers to according to ammonium ion concentration in tested pretreatment sample solution, by member
Plain law of conservation, is computed obtaining the percentage composition of cyanic acid ion in tested solid-based salt sample.
Claims (10)
1. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument, including flow path system, specimen inspection system,
Embedded Webserver；It is characterized in that：The flow path system includes multiposition valve (1), syringe pump (2), pipeline；Flow path system point
Lian Jie not sample, detection reagent, distilled water, sample conversion reaction pond (8), the multiposition valve (1), syringe pump (2) connection
Embedded Webserver；
The specimen inspection system includes LED light source, sample detection room (7), photodiode, and the LED light source is saturating through first
Mirror (13) collimates emitting parallel light, through sample detection room (7), then is focused on by the second lens (14) into photodiode
Optical window, is directly translated into photovoltage output；
The embedded Webserver includes power module (16), and embedded Webserver sends control command by serial ports, controls
Flow path system processed, specimen inspection system, while obtaining the data of specimen inspection system output by serial ports and dealing with analysis.
2. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 1, its feature exists
In：The multiposition valve (1) has multi-channel flow passage handoff functionality, and its common port (4) connects liquid storage ring (5) one by PEEK pipes
End, a flow path channel of liquid storage ring (5) other end connection syringe pump (2), another changeable stream of syringe pump (2)
Passage connects distilled water pond (6) by PEEK pipes.
3. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 1, its feature exists
In：The sample conversion reaction pond (8) includes stainless steel sealed taper shaped reaction room (9), constant temperature water bath pond (10), multiposition valve (1)
Valve position 11# pass through PEEK pipes connection sample detection room (7)；The valve position 9# of the multiposition valve (1) connects sample by PEEK pipes
The stainless steel sealed taper shaped reaction room (9) in conversion reaction pond (8)；The valve position 10# of the multiposition valve (1) connects sample by PEEK pipes
The constant temperature water bath pond (10) in product conversion reaction pond (8)；The valve position 8# connection waste liquid pools (12) of the multiposition valve (1).
4. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 3, its feature exists
In：Constant temperature water bath pond (10) material is stainless steel, its bottom integrated heating pipe (11), for adding to sample conversion reaction
Heat, when reaction system is freezed, heating tube (11) power-off.
5. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 1, its feature exists
In：The sample detection room (7) includes aluminium cell body (20), the cuvette (19) being mounted in aluminium cell body (20), than
Color cup (19) is quartz glass material, and aluminium cell body (20) bottom installs heating rod (21), passes through temperature control and air
Heat transfer, realizes the thermostatic control of contrastive colours cup (19) interior reaction solution.
6. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 5, its feature exists
In：Photoelectric Detection module is equipped with the aluminium cell body (20)：Light emitting diode (22) and photodiode (23), the hair
The detection light beam (24) that optical diode (22) is sent is through the example reaction solution in cuvette (19), into photodiode
(23), through opto-electronic conversion, sample concentration is detected by absorption spectroanalysis.
7. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 1, its feature exists
In：The embedded Webserver includes power module (16), embedded processing module (15), peripheral control circuits (17), number
According to Acquisition Circuit (18)；
Embedded processing module (15) the connection peripheral control circuits (17), peripheral control circuits (17) are used to realize that light source drives
Dynamic control, stream control, temperature control；
Embedded processing module (15) the connection data acquisition circuit (18), data acquisition circuit (18) passes through Signal Regulation electricity
Road (28) connects photodiode.
8. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument according to claim 7, its feature exists
In：The embedded processing module (15) is connected with man-machine interactive system by serial ports, and man-machine interactive system includes memory
(29), touch-control LCD display (25) and gprs system (26), gprs system (26) is by being wirelessly transferred with host computer (27) even
Connect.
9. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analysis method, it is characterised in that：Cyanate content detection is adopted
With Indirect Detecting Method, first pass through chemical method and cyanate radical CNO- is changed into ammonium root NH4+, as shown in (1) formula, then according to mark
Quasi- GB7481-1987：The measure salicylic acid AAS of water quality ammonium, by the measure to ammonium ion, detection characteristic wavelength is
697nm, realizes the detection to cyanate content indirectly.
10. a kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analysis method, it is characterised in that：
(1) demarcate：The ammonium chloride standard sample solution of respective concentration gradient is prepared with distilled water, with standard sample solution replacement quilt
Salt sample Solutions Solution, control syringe pump (2) and multiposition valve (1) are surveyed, standard sample solution and the corresponding bigcatkin willow of certain volume
2. 1. acid reagent is pumped into liquid storage ring (5) successively with bigcatkin willow acid reagent, and then the rotor of multiposition valve 1 goes to valve position 11#, syringe pump
(2) it is counter to push away, standard sample solution and reaction reagent push-in sample detection room (7), colour developing is completed in sample detection room (7) anti-
The absorbance A of reaction system and should be detected, with the concentration C abscissa of standard liquid, using corresponding absorbance A as ordinate, profit
Standard working curve is fitted with the principle of least square, standard working curve is cured to embedded Webserver；
(2) detect：For tested base salt sample solution, first completed in sample conversion reaction pond (8) after sample conversion, sample
2. 1. the preprocessing solution of conversion reaction pond (8) interior certain volume be pumped into successively with corresponding bigcatkin willow acid reagent with bigcatkin willow acid reagent
In liquid storage ring (5), then multiposition valve (1) rotor goes to valve position 11#, and syringe pump (2) is counter to be pushed away, preprocessing solution and reaction reagent
It is pushed into sample detection room (7), chromogenic reaction is completed inside and absorbance A is detected, absorbance A is finally substituted into standard working curve
The concentration of ammonium root in sample can be calculated, the content of cyanate in sample is thus being calculated indirectly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710213660.1A CN106959350A (en) | 2017-04-01 | 2017-04-01 | A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710213660.1A CN106959350A (en) | 2017-04-01 | 2017-04-01 | A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106959350A true CN106959350A (en) | 2017-07-18 |
Family
ID=59484863
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710213660.1A Pending CN106959350A (en) | 2017-04-01 | 2017-04-01 | A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106959350A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956517A (en) * | 2018-09-11 | 2018-12-07 | 哈尔滨工业大学 | A kind of real-time online continuously monitors the device and its application method of sulfate concentration |
| CN109238996A (en) * | 2018-09-11 | 2019-01-18 | 哈尔滨工业大学 | A kind of real-time online continuously monitors the device and its application method of nitrate concentration |
| CN110161164A (en) * | 2019-04-16 | 2019-08-23 | 大连诚泽检测有限公司 | A kind of flow-type stoichiometric point measurement device and its application |
| CN114778761A (en) * | 2022-04-20 | 2022-07-22 | 西安近代化学研究所 | QPQ process radical cyanate content determination device and method |
| CN115711964A (en) * | 2022-11-29 | 2023-02-24 | 北京泊菲莱科技有限公司 | Flow type photocatalytic rapid detection system and application method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204462005U (en) * | 2015-04-08 | 2015-07-08 | 三峡大学 | A kind of water quality heavy metal on-line sample detection system |
| CN104764696A (en) * | 2015-04-08 | 2015-07-08 | 三峡大学 | Water quality heavy metal online sample detection system |
| CN204536343U (en) * | 2015-04-08 | 2015-08-05 | 三峡大学 | A kind of water quality heavy metal multiparameter on-line monitoring instrument |
| CN105954218A (en) * | 2016-06-27 | 2016-09-21 | 魏康林 | Semiautomatic QPQ-process-oriented nitride salt component detection instrument |
| CN206638640U (en) * | 2017-04-01 | 2017-11-14 | 三峡大学 | A kind of QPQ technologies base salt cyanic acid radical content automatically tests and analyzes instrument |
-
2017
- 2017-04-01 CN CN201710213660.1A patent/CN106959350A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204462005U (en) * | 2015-04-08 | 2015-07-08 | 三峡大学 | A kind of water quality heavy metal on-line sample detection system |
| CN104764696A (en) * | 2015-04-08 | 2015-07-08 | 三峡大学 | Water quality heavy metal online sample detection system |
| CN204536343U (en) * | 2015-04-08 | 2015-08-05 | 三峡大学 | A kind of water quality heavy metal multiparameter on-line monitoring instrument |
| CN105954218A (en) * | 2016-06-27 | 2016-09-21 | 魏康林 | Semiautomatic QPQ-process-oriented nitride salt component detection instrument |
| CN206638640U (en) * | 2017-04-01 | 2017-11-14 | 三峡大学 | A kind of QPQ technologies base salt cyanic acid radical content automatically tests and analyzes instrument |
Non-Patent Citations (1)
| Title |
|---|
| 魏康林;周丰;王振帅;戴贤明;胡滨;余丽;谭森;: "在线水质监测仪流路系统及其控制电路设计" * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956517A (en) * | 2018-09-11 | 2018-12-07 | 哈尔滨工业大学 | A kind of real-time online continuously monitors the device and its application method of sulfate concentration |
| CN109238996A (en) * | 2018-09-11 | 2019-01-18 | 哈尔滨工业大学 | A kind of real-time online continuously monitors the device and its application method of nitrate concentration |
| CN110161164A (en) * | 2019-04-16 | 2019-08-23 | 大连诚泽检测有限公司 | A kind of flow-type stoichiometric point measurement device and its application |
| CN114778761A (en) * | 2022-04-20 | 2022-07-22 | 西安近代化学研究所 | QPQ process radical cyanate content determination device and method |
| CN114778761B (en) * | 2022-04-20 | 2023-09-08 | 西安近代化学研究所 | QPQ process base salt cyanate radical content determination device and method |
| CN115711964A (en) * | 2022-11-29 | 2023-02-24 | 北京泊菲莱科技有限公司 | Flow type photocatalytic rapid detection system and application method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106959350A (en) | A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument | |
| Mazarevica et al. | On-line fermentation monitoring by mid-infrared spectroscopy | |
| CN102147373B (en) | Multi-parameter water quality monitoring system based on micro-optical-electro-mechanical system (MOEMS) micro spectrometer | |
| CN101320001A (en) | High pressure flow injection rapid analysis system for permanganate index of water quality | |
| CN105388309A (en) | Automatic and rapid detection method and system for trace iron ions in power plant water vapor and application | |
| CN211877738U (en) | Spectrophotometric assay and liquid handling system | |
| CN204128953U (en) | Auto injection gas phase molecular absorption spectrometer | |
| CN110132916B (en) | Accurate quantitative analysis method for metal elements | |
| CN104034670A (en) | Dual-index water quality on-line analysis method and apparatus for simultaneous determination of COD and ammonia nitrogen | |
| CN101587109B (en) | Determination method and intruments of hexavalent chromium | |
| CN108051037A (en) | A kind of syringe pump flow calibrating device and calibration method | |
| CN210222042U (en) | Online intelligent air quality formaldehyde tester | |
| CN100501377C (en) | Device for quickly identifying age of Chinese rice wine based on near infrared spectrum | |
| CN100422718C (en) | Method for determining sodium chloride content in phosphate using spectrophotometry | |
| CN205080143U (en) | Automatic quick detecting system of trace iron ion in power plant's steam | |
| CN206638640U (en) | A kind of QPQ technologies base salt cyanic acid radical content automatically tests and analyzes instrument | |
| Jiménez-Márquez et al. | High-resolution low-cost optoelectronic instrument for supervising grape must fermentation | |
| CN105954218B (en) | A kind of semi-automatic detecting instrument of nitridation salt component towards QPQ techniques | |
| CN205826527U (en) | A kind of semi-automatic detecting instrument of nitridation salt composition towards QPQ technique | |
| CN110006893B (en) | Online automatic determination method for zirconium silane concentration | |
| CN206020441U (en) | The measurement apparatus measured using standard addition method | |
| RU154434U1 (en) | SYSTEM FOR ANALYSIS OF COMPOSITIONS OF GAS AND / OR LIQUID TECHNOLOGICAL FLOWS OF CHEMICAL PRODUCTION | |
| US10222322B2 (en) | Colorimetric analyzer with improved error detection | |
| CN2110225U (en) | Semi-automatic biochemistry analysis instrument | |
| CN1740773A (en) | Double-light path seawater phosphate optical analyzing system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |