CN112378868A - Method for detecting content of metal components in polyphenylene sulfide - Google Patents
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a method for detecting the content of metal components in polyphenylene sulfide, relates to the technical field of polyphenylene sulfide detection, and aims to solve the problems that the detection of the content of the metal components in the conventional polyphenylene sulfide is usually completed by a spectrophotometry, but a spectrophotometer is complicated to use, a sample needs to be manually placed and taken, the content of the sample is controlled, and the detection efficiency is seriously influenced. Step 1: weighing a proper amount of polyphenylene sulfide powder, mixing the polyphenylene sulfide powder with sulfuric acid for reaction, heating and carbonizing, and digesting with nitric acid to prepare a sample digestion solution; step 2: plugging a power supply of a spectrophotometer, opening a switch and a cover of a sample chamber, and preheating for 30 minutes; and step 3: preparing eight colorimetric tubes, placing the colorimetric tubes on the supporting through holes in the sample tray after the eight colorimetric tubes are washed by the reference solution, and closing the cover of the sample chamber.
Description
Technical Field
The invention relates to the technical field of polyphenylene sulfide detection, in particular to a method for detecting the content of metal components in polyphenylene sulfide.
Background
Polyphenylene Sulfide (PPS), abbreviated as English, is a novel high-performance thermoplastic resin and has the advantages of high mechanical strength, high temperature resistance, chemical resistance, flame retardancy, good thermal stability, excellent electrical property and the like. The polyphenylene sulfide is a special engineering plastic with excellent comprehensive performance, and the PPS has the characteristics of excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardance, static resistance, balanced physical and mechanical properties, excellent dimensional stability, excellent electrical property and the like, is widely used as a structural high polymer material, and is widely used as a special engineering plastic after being filled and modified. Meanwhile, the composite material can be made into various functional films, coatings and composite materials, and can be successfully applied to the fields of electronic appliances, aerospace, automobile transportation and the like.
The existing polyphenylene sulfide metal component content detection is usually completed by adopting a spectrophotometry method, but the use of a spectrophotometer is more complicated, samples need to be manually placed and taken, the content of the samples is controlled, and the detection efficiency is seriously influenced; therefore, the existing requirements are not met, and a method for detecting the content of the metal component in the polyphenylene sulfide is provided for the requirements.
Disclosure of Invention
The invention aims to provide a method for detecting the content of metal components in polyphenylene sulfide, which aims to solve the problems that the detection efficiency is seriously influenced because the conventional method for detecting the content of the metal components in the polyphenylene sulfide is generally completed by adopting a spectrophotometry, but a spectrophotometer is complicated to use, and a sample needs to be manually placed and taken to control the content of the sample.
In order to achieve the purpose, the invention provides the following technical scheme: the method for detecting the content of the metal components in the polyphenylene sulfide comprises the following steps:
step 1: weighing a proper amount of polyphenylene sulfide powder, mixing the polyphenylene sulfide powder with sulfuric acid for reaction, heating and carbonizing, and digesting with nitric acid to prepare a sample digestion solution;
step 2: plugging a power supply of a spectrophotometer, opening a switch and a cover of a sample chamber, and preheating for 30 minutes;
and step 3: preparing eight colorimetric tubes, placing the colorimetric tubes on the supporting through holes in the sample tray after the eight colorimetric tubes are wetted by reference liquid, and closing a cover of the sample chamber;
and 4, step 4: pouring the digestion solution into a digestion solution storage chamber in the spectrophotometer, starting a metering pump, quantitatively pumping the digestion solution into a colorimetric tube at the lower end of an injection nozzle, and loading a sample into the colorimetric tube 3/4;
and 5: after the first colorimetric tube is filled, driving a stepping motor to drive a sample disc to rotate by forty-five degrees, switching to the next colorimetric tube, starting the metering pump again, and repeating the steps until the filling work of the eight colorimetric tubes is completed;
step 6: after the sample is loaded, selecting the wavelength of the metal substance to be measured, pressing a mode key of the device, and selecting a T%' state, so as to detect the colorimetric tube at the front end through the light path;
and 7: after the detection of the color comparison tubes is finished, driving a stepping motor to drive the sample plate to rotate by forty-five degrees, and switching to the next color comparison tube for detection until the detection work of eight groups of color comparison tubes is finished;
and 8: recording detection data, taking out the colorimetric tube, pouring out digestion solution, reloading the digestion solution into the sample tray, and cleaning the equipment;
wherein, the spectrophotometer comprises a spectrophotometer main body, a parameter panel is installed at the upper end of the spectrophotometer main body, a wavelength adjusting knob is arranged at the front end of the parameter panel, a sample chamber cover is installed on the upper surface of the spectrophotometer main body, a digestion solution storage chamber is installed on one side of the spectrophotometer main body, an auxiliary power chamber is arranged at the lower end of the digestion solution storage chamber, a metering pump is installed at the rear end of the digestion solution storage chamber, a sample chamber is arranged in the spectrophotometer main body, a main power chamber is arranged at the lower end of the sample chamber, a sample disc is arranged in the sample chamber, bearing through holes are arranged on the sample disc, six bearing through holes are arranged, a connecting seat is installed at the lower end of the sample disc, a coupler is installed at the lower end of the connecting seat, and a stepping motor is installed in the main power chamber, step motor's output runs through and extends to the inside of sample room, and is connected with the connecting seat transmission through the shaft coupling, one side of step motor is provided with the ultrasonic frequency power, ultrasonic transducer is all installed to the upper surface of main power room and vice power room, first drain valve is installed to the front end of sample room, the second drain valve is installed to one side of digestion liquid locker room, the liquid feeding fill is installed to the upper end of digestion liquid locker room, the hopper lid is installed to the upper end of liquid feeding fill, and the hopper lid rotates with the liquid feeding fill to be connected, be provided with the heat dissipation tripe on the preceding terminal surface of main power room, and the heat dissipation tripe is provided with nine
Preferably, the polyphenylene sulfide digestion reaction in the step 1 specifically comprises:
step 1-1: pouring a proper amount of polyphenylene sulfide powder into a vacuum heating tank, adding a proper amount of sulfuric acid, mixing and reacting, extracting air in the tank to enable the polyphenylene sulfide powder to be in a vacuum-pumping state, heating the polyphenylene sulfide powder to 400 ℃, and keeping the temperature for 30 minutes to enable the polyphenylene sulfide powder to be carbonized;
step 1-2: after carbonization, regulating the temperature to 250 ℃ again, slowly adding the nitric acid digestion solution into the tank, checking the condition of the content solution through an observation window during digestion, and obtaining a clear state;
step 1-3: and opening a valve of the vacuum heating tank, and taking out the digestion solution for later use.
Preferably, in the step 1-1, the proportioning concentration of the polyphenylene sulfide powder and the sulfuric acid is 0.05 g/ml.
Preferably, in the step 8, the cleaning method of the device specifically includes:
step 8-1: firstly, discharging the digestion solution in the digestion solution storage chamber through a drain valve, pouring a proper amount of clear water into the digestion solution storage chamber and the sample chamber, wherein the clear water in the sample chamber should submerge a colorimetric tube inside;
step 8-2: starting an ultrasonic frequency power supply, driving an ultrasonic transducer to operate to emit ultrasonic radiation, enabling clear water in the tank to generate micro bubbles and keep vibrating, and destroying stains on the inner wall of the digestion solution storage chamber and the colorimetric tube, so that the effect of efficient cleaning is achieved;
step 8-3: after the cleaning is finished, the sewage in the digestion liquid storage chamber and the sample chamber is discharged through the drain valve.
Preferably, a liquid suction pipe is installed on the water inlet end of the metering pump, one end of the liquid suction pipe penetrates through and extends to the interior of the digestion liquid storage chamber, a liquid discharge pipe is installed on the water outlet end of the metering pump, one end of the liquid discharge pipe penetrates through and extends to the interior of the cover of the specimen chamber, and an injection nozzle is installed at one end of the liquid discharge pipe.
Preferably, the central point of the injection nozzle coincides with the central point of the supporting through hole.
Preferably, the output end of the ultrasonic frequency power supply is electrically connected with the input end of the ultrasonic transducer.
Preferably, a mechanical seal is installed at the connection position of the output end of the stepping motor and the sample chamber.
Preferably, the lower surface mounting of spectrophotometer main part has the shock attenuation callus on the sole, and the shock attenuation callus on the sole is provided with eight.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the digestion solution is quantitatively pumped into the colorimetric tube at the lower end of the injection nozzle by adopting the metering pump, and after the sample loading of the colorimetric tube right below the injection nozzle is finished, the stepper motor is driven to drive the sample plate to rotate by forty-five degrees, so that the sample can be switched to the next colorimetric tube, the sample loading work of eight colorimetric tubes can be completed at most once, the comparison test is convenient to carry out, the detection accuracy is improved, compared with the detection of a conventional spectrophotometer, the manual sample loading is not needed, and the detection efficiency is greatly improved.
2. Bear the colour comparison tube through adopting the sample dish, the lower extreme of sample dish is connected with step motor's output transmission, and during the detection, the light path can be preferred to be detected just to its colour comparison tube sample, treats to reachs the testing result after, starts step motor and drives sample dish rotation forty-five degrees, can switch to next sample and detect, compares with current spectrophotometry detection, need not artifical manual push-and-pull colour comparison frame pull rod, and it is more convenient to use.
3. Through the last surface mounting ultrasonic transducer at main power room and vice power room, ultrasonic transducer relies on the ultrasonic frequency power supply, can send ultrasonic wave radiation during the operation, makes the inslot clear water produce the microbubble and keep vibrating, destroys the spot on digestion liquid storage chamber inner wall and the colour comparison tube to reach high-efficient abluent effect, conveniently carry out next detection fast.
Drawings
FIG. 1 is a schematic view showing the process of detecting the content of metal components in polyphenylene sulfide according to the present invention;
FIG. 2 is a schematic view of a spectrophotometer cleaning process of the present invention;
FIG. 3 is a schematic structural view of the present invention;
FIG. 4 is a schematic structural view of the present invention;
FIG. 5 is a schematic structural view of the present invention;
in the figure: 1. a spectrophotometer main body; 2. a parameter panel; 3. a wavelength adjusting knob; 4. a sample chamber cover; 5. a first drain valve; 6. a digestion liquid storage chamber; 7. a second drain valve; 8. a shock-absorbing foot pad; 9. a liquid inlet hopper; 10. a hopper cover; 11. a metering pump; 12. a pipette; 13. a liquid discharge pipe; 14. a sample chamber; 15. an optical path; 16. a sample tray; 161. supporting the through hole; 17. an injection nozzle; 18. a connecting seat; 19. a coupling; 20. a main power chamber; 21. a stepping motor; 22. a mechanical seal; 23. an ultrasonic frequency power supply; 24. a secondary power chamber; 25. an ultrasonic transducer; 26. the heat dissipation louver.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, an embodiment of the present invention is shown: the method for detecting the content of the metal components in the polyphenylene sulfide comprises the following steps:
step 1: weighing a proper amount of polyphenylene sulfide powder, mixing the polyphenylene sulfide powder with sulfuric acid for reaction, heating and carbonizing, and digesting with nitric acid to prepare a sample digestion solution;
step 2: plugging a power supply of a spectrophotometer, opening a switch and a cover of a sample chamber, and preheating for 30 minutes;
and step 3: preparing eight colorimetric tubes, placing the colorimetric tubes on the supporting through holes in the sample tray after the eight colorimetric tubes are wetted by reference liquid, and closing a cover of the sample chamber;
and 4, step 4: pouring the digestion solution into a digestion solution storage chamber in the spectrophotometer, starting a metering pump, quantitatively pumping the digestion solution into a colorimetric tube at the lower end of an injection nozzle, and loading a sample into the colorimetric tube 3/4;
and 5: after the first colorimetric tube is filled, driving a stepping motor to drive a sample disc to rotate by forty-five degrees, switching to the next colorimetric tube, starting the metering pump again, and repeating the steps until the filling work of the eight colorimetric tubes is completed;
step 6: after the sample is loaded, selecting the wavelength of the metal substance to be measured, pressing a mode key of the device, and selecting a T%' state, so as to detect the colorimetric tube at the front end through the light path;
and 7: after the detection of the color comparison tubes is finished, driving a stepping motor to drive the sample plate to rotate by forty-five degrees, and switching to the next color comparison tube for detection until the detection work of eight groups of color comparison tubes is finished;
and 8: recording detection data, taking out the colorimetric tube, pouring out digestion solution, reloading the digestion solution into the sample tray, and cleaning the equipment;
wherein, the spectrophotometer comprises a spectrophotometer main body 1, the internal detection element of the spectrophotometer main body 1 is based on the instrument structure of 721 type spectrophotometer, a parameter panel 2 is installed at the upper end of the spectrophotometer main body 1, a wavelength adjusting knob 3 is arranged at the front end of the parameter panel 2, a sample chamber cover 4 is installed on the upper surface of the spectrophotometer main body 1, a digestion solution storage chamber 6 is installed at one side of the spectrophotometer main body 1, an auxiliary power chamber 24 is arranged at the lower end of the digestion solution storage chamber 6, a metering pump 11 is installed at the rear end of the digestion solution storage chamber 6, a sample chamber 14 is arranged in the spectrophotometer main body 1, a main power chamber 20 is arranged at the lower end of the sample chamber 14, a sample disc 16 is arranged in the sample chamber 14, a bearing through hole 161 is arranged on the sample disc 16, six bearing through holes 161 are arranged, a connecting seat 18 is installed at the, coupling 19 is installed to the lower extreme of connecting seat 18, the internally mounted of main power room 20 has step motor 21, step motor 21's output runs through and extends to the inside of sample room 14, and be connected with connecting seat 18 transmission through coupling 19, one side of step motor 21 is provided with ultrasonic frequency power 23, ultrasonic transducer 25 is all installed to the upper surface of main power room 20 and vice power room 24, first drain valve 5 is installed to the front end of sample room 14, second drain valve 7 is installed to one side of digestion liquid locker room 6, feed hopper 9 is installed to the upper end of digestion liquid locker room 6, hopper lid 10 is installed to the upper end of feed hopper 9, and hopper lid 10 rotates with feed hopper 9 to be connected, be provided with heat dissipation tripe 26 on the front end face of main power room 20, and heat dissipation tripe 26 is provided with nine
Further, the polyphenylene sulfide digestion reaction in the step 1 specifically comprises:
step 1-1: pouring a proper amount of polyphenylene sulfide powder into a vacuum heating tank, adding a proper amount of sulfuric acid, mixing and reacting, extracting air in the tank to enable the polyphenylene sulfide powder to be in a vacuum-pumping state, heating the polyphenylene sulfide powder to 400 ℃, and keeping the temperature for 30 minutes to enable the polyphenylene sulfide powder to be carbonized;
step 1-2: after carbonization, regulating the temperature to 250 ℃ again, slowly adding the nitric acid digestion solution into the tank, checking the condition of the content solution through an observation window during digestion, and obtaining a clear state;
step 1-3: and opening a valve of the vacuum heating tank, and taking out the digestion solution for later use.
Further, in the step 1-1, the proportioning concentration of the polyphenylene sulfide powder and the sulfuric acid is 0.05 g/ml.
Further, in step 8, the method for cleaning the equipment specifically comprises the following steps:
step 8-1: firstly, discharging the digestion solution in the digestion solution storage chamber through a drain valve, pouring a proper amount of clear water into the digestion solution storage chamber and the sample chamber, wherein the clear water in the sample chamber should submerge a colorimetric tube inside;
step 8-2: starting an ultrasonic frequency power supply, driving an ultrasonic transducer to operate to emit ultrasonic radiation, enabling clear water in the tank to generate micro bubbles and keep vibrating, and destroying stains on the inner wall of the digestion solution storage chamber and the colorimetric tube, so that the effect of efficient cleaning is achieved;
step 8-3: after the cleaning is finished, the sewage in the digestion liquid storage chamber and the sample chamber is discharged through the drain valve.
Further, install pipette 12 on the intake of measuring pump 11, and the one end of pipette 12 runs through and extends to the inside in digestion liquid locker room 6, install fluid-discharge tube 13 on the play water end of measuring pump 11, and the one end of fluid-discharge tube 13 runs through and extends to the inside of apotheca cover 4, injection nozzle 17 is installed to the one end of fluid-discharge tube 13, measuring pump 11 can be with in the digestion liquid sample ration pump in the digestion liquid locker room 6 go into the colour comparison tube in the apotheca 14, realize automatic dress appearance.
Further, the center point of the injection nozzle 17 coincides with the center point of the bearing through hole 161, so that the injection precision is ensured, and after the sample loading work of the lower colorimetric tube is completed, the sample tray 16 can be driven by the stepping motor 21 to rotate by forty-five degrees, and then the sample tray is switched to the next colorimetric tube to continue to load the sample.
Further, the output end of the ultrasonic frequency power supply 23 is electrically connected with the input end of the ultrasonic transducer 25, and the ultrasonic frequency power supply can drive the ultrasonic transducer to operate to emit ultrasonic radiation, so that the effect of ultrasonic cleaning equipment is achieved.
Further, mechanical seal 22 is installed at the junction of the output end of stepping motor 21 and sample chamber 14, and mechanical seal 22 ensures the sealing performance of the junction of stepping motor 21 and sample chamber 14, and avoids water from permeating from the junction gap during cleaning.
Further, the lower surface mounting of spectrophotometer main part 1 has shock attenuation callus on the sole 8, and shock attenuation callus on the sole 8 is provided with eight, and shock attenuation callus on the sole 8 is for having the rubber material of anti-skidding line, can guarantee the stability when equipment moves.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The method for detecting the content of the metal components in the polyphenylene sulfide is characterized by comprising the following steps:
step 1: weighing a proper amount of polyphenylene sulfide powder, mixing the polyphenylene sulfide powder with sulfuric acid for reaction, heating and carbonizing, and digesting with nitric acid to prepare a sample digestion solution;
step 2: plugging a power supply of a spectrophotometer, opening a switch and a cover of a sample chamber, and preheating for 30 minutes;
and step 3: preparing eight colorimetric tubes, placing the colorimetric tubes on the supporting through holes in the sample tray after the eight colorimetric tubes are wetted by reference liquid, and closing a cover of the sample chamber;
and 4, step 4: pouring the digestion solution into a digestion solution storage chamber in the spectrophotometer, starting a metering pump, quantitatively pumping the digestion solution into a colorimetric tube at the lower end of an injection nozzle, and loading a sample into the colorimetric tube 3/4;
and 5: after the first colorimetric tube is filled, driving a stepping motor to drive a sample disc to rotate by forty-five degrees, switching to the next colorimetric tube, starting the metering pump again, and repeating the steps until the filling work of the eight colorimetric tubes is completed;
step 6: after the sample is loaded, selecting the wavelength of the metal substance to be measured, pressing a mode key of the device, and selecting a T%' state, so as to detect the colorimetric tube at the front end through the light path;
and 7: after the detection of the color comparison tubes is finished, driving a stepping motor to drive the sample plate to rotate by forty-five degrees, and switching to the next color comparison tube for detection until the detection work of eight groups of color comparison tubes is finished;
and 8: recording detection data, taking out the colorimetric tube, pouring out digestion solution, reloading the digestion solution into the sample tray, and cleaning the equipment;
wherein, spectrophotometer includes spectrophotometer main part (1), parameter panel (2) are installed to the upper end of spectrophotometer main part (1), the front end of parameter panel (2) is provided with wavelength adjust knob (3), the last surface mounting of spectrophotometer main part (1) has sample room cover (4), digest liquid locker room (6) is installed to one side of spectrophotometer main part (1), the lower extreme of digest liquid locker room (6) is provided with vice power room (24), measuring pump (11) is installed to the rear end of digest liquid locker room (6), the inside of spectrophotometer main part (1) is provided with sample room (14), the lower extreme of sample room (14) is provided with main power room (20), the inside of sample room (14) is provided with sample dish (16), be provided with bearing through-hole (161) on sample dish (16), and bearing through hole (161) is provided with six, connecting seat (18) are installed to the lower extreme of sample dish (16), shaft coupling (19) are installed to the lower extreme of connecting seat (18), the internally mounted of main power room (20) has step motor (21), the output of step motor (21) runs through and extends to the inside of sample room (14), and is connected with connecting seat (18) transmission through shaft coupling (19), one side of step motor (21) is provided with ultrasonic frequency power (23), ultrasonic transducer (25) are all installed to the upper surface of main power room (20) and auxiliary power room (24), first drain valve (5) are installed to the front end of sample room (14), second drain valve (7) are installed to one side of digestion liquid locker room (6), liquid feeding fill (9) are installed to the upper end of digestion liquid locker room (6), hopper cover (10) are installed to the upper end of feed liquor fill (9), and hopper cover (10) rotate with feed liquor fill (9) and be connected, be provided with heat dissipation tripe (26) on the preceding terminal surface of main power room (20), and heat dissipation tripe (26) are provided with nine.
2. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein the polyphenylene sulfide digestion reaction in the step 1 is specifically:
step 1-1: pouring a proper amount of polyphenylene sulfide powder into a vacuum heating tank, adding a proper amount of sulfuric acid, mixing and reacting, extracting air in the tank to enable the polyphenylene sulfide powder to be in a vacuum-pumping state, heating the polyphenylene sulfide powder to 400 ℃, and keeping the temperature for 30 minutes to enable the polyphenylene sulfide powder to be carbonized;
step 1-2: after carbonization, regulating the temperature to 250 ℃ again, slowly adding the nitric acid digestion solution into the tank, checking the condition of the content solution through an observation window during digestion, and obtaining a clear state;
step 1-3: and opening a valve of the vacuum heating tank, and taking out the digestion solution for later use.
3. The method for detecting the content of the metal component in the polyphenylene sulfide according to claim 2, wherein: in the step 1-1, the proportioning concentration of the polyphenylene sulfide powder and the sulfuric acid is 0.05 g/ml.
4. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein in the step 8, the equipment cleaning method specifically comprises:
step 8-1: firstly, discharging the digestion solution in the digestion solution storage chamber through a drain valve, pouring a proper amount of clear water into the digestion solution storage chamber and the sample chamber, wherein the clear water in the sample chamber should submerge a colorimetric tube inside;
step 8-2: starting an ultrasonic frequency power supply, driving an ultrasonic transducer to operate to emit ultrasonic radiation, enabling clear water in the tank to generate micro bubbles and keep vibrating, and destroying stains on the inner wall of the digestion solution storage chamber and the colorimetric tube, so that the effect of efficient cleaning is achieved;
step 8-3: after the cleaning is finished, the sewage in the digestion liquid storage chamber and the sample chamber is discharged through the drain valve.
5. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein: install pipette (12) on the water inlet end of measuring pump (11), and the one end of pipette (12) runs through and extends to the inside of digestion liquid locker room (6), install fluid-discharge tube (13) on the water outlet end of measuring pump (11), and the one end of fluid-discharge tube (13) runs through and extends to the inside of apotheca cover (4), injection nozzle (17) are installed to the one end of fluid-discharge tube (13).
6. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 5, wherein: the central point of the injection nozzle (17) is coincided with the central point of the bearing through hole (161).
7. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein: the output end of the ultrasonic frequency power supply (23) is electrically connected with the input end of the ultrasonic transducer (25).
8. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein: and a mechanical sealing element (22) is arranged at the joint of the output end of the stepping motor (21) and the sample chamber (14).
9. The method for detecting the content of the metal component in the polyphenylene sulfide as claimed in claim 1, wherein: the lower surface mounting of spectrophotometer main part (1) has shock attenuation callus on the sole (8), and shock attenuation callus on the sole (8) are provided with eight.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102313706A (en) * | 2011-05-30 | 2012-01-11 | 广东工业大学 | Digestion and determination method of heavy metals in waste dust-collecting bag |
| CN103439315A (en) * | 2013-09-06 | 2013-12-11 | 方玉枝 | Method for detecting mercury content in polymeric material and sample processing method |
| CN204255850U (en) * | 2014-12-11 | 2015-04-08 | 周口师范学院 | A kind of ultraviolet spectrophotometer |
| CN106872384A (en) * | 2017-04-07 | 2017-06-20 | 北京瀚时仪器有限公司 | A kind of high-efficiency atomizer for atomic absorption spectrophotometer |
| CN208537402U (en) * | 2018-07-19 | 2019-02-22 | 郑州市通标环境检测有限公司 | A kind of rapid-digestion spectrophotometer method detection device |
| CN210742118U (en) * | 2019-08-27 | 2020-06-12 | 武汉俊德环保科技发展有限公司 | Automatic color comparison device of quality of water |
-
2020
- 2020-10-16 CN CN202011108973.9A patent/CN112378868B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102313706A (en) * | 2011-05-30 | 2012-01-11 | 广东工业大学 | Digestion and determination method of heavy metals in waste dust-collecting bag |
| CN103439315A (en) * | 2013-09-06 | 2013-12-11 | 方玉枝 | Method for detecting mercury content in polymeric material and sample processing method |
| CN204255850U (en) * | 2014-12-11 | 2015-04-08 | 周口师范学院 | A kind of ultraviolet spectrophotometer |
| CN106872384A (en) * | 2017-04-07 | 2017-06-20 | 北京瀚时仪器有限公司 | A kind of high-efficiency atomizer for atomic absorption spectrophotometer |
| CN208537402U (en) * | 2018-07-19 | 2019-02-22 | 郑州市通标环境检测有限公司 | A kind of rapid-digestion spectrophotometer method detection device |
| CN210742118U (en) * | 2019-08-27 | 2020-06-12 | 武汉俊德环保科技发展有限公司 | Automatic color comparison device of quality of water |
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