CN112014386A - Method for detecting content of trace iron in quartz sand - Google Patents
Method for detecting content of trace iron in quartz sand Download PDFInfo
- Publication number
- CN112014386A CN112014386A CN202010819422.7A CN202010819422A CN112014386A CN 112014386 A CN112014386 A CN 112014386A CN 202010819422 A CN202010819422 A CN 202010819422A CN 112014386 A CN112014386 A CN 112014386A
- Authority
- CN
- China
- Prior art keywords
- cooling chamber
- reagent
- iron
- bottle
- electromagnet
- 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
Images
Classifications
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
Abstract
The invention discloses a method for detecting the content of trace iron in quartz sand, which belongs to the technical field of quartz sand treatment and comprises the following steps: preparing a sample to be tested: weighing siliceous sandstone, putting the siliceous sandstone into a polytetrafluoroethylene bottle, adding concentrated hydrofluoric acid, putting the bottle into a microwave oven, taking out the bottle after the siliceous sandstone is completely decomposed, and cooling the bottle to obtain a sample to be detected; presetting a Fe reagent 2: weighing 0.6g of Fe reagent 2, putting the Fe reagent 2 into a 30ml lightproof plastic bottle, adding ethanol and water, and shaking until the Fe reagent 2 is completely dissolved to obtain a preset Fe reagent 2; presetting a Fe reagent 1: measuring 10ml of Fe reagent 1, and adding 3 drops of 3% ascorbic acid to obtain a preset Fe reagent 1; color development and measurement: and (4) adding 0.2ml of the preset Fe reagent 2 into the preset Fe reagent 1 obtained in the step (S3), shaking up, adding a sample to be measured, shaking up, and measuring by using a measuring instrument.
Description
Technical Field
The invention relates to the technical field of quartz sand treatment, in particular to a method for detecting the content of trace iron in quartz sand.
Background
The quartz sand is quartz particles formed by crushing and processing quartz stone, is a non-metallic mineral substance, and is a silicate mineral with hardness, wear resistance and stable chemical properties. The quartz sand is milky white or colorless and semitransparent, and has a Mohs hardness of 7. Quartz sand is an important industrial mineral raw material and a non-chemical hazardous article, and is widely used in the industries of glass, casting, ceramics and fireproof materials, ferrosilicon smelting, metallurgical flux, metallurgy, building, chemical engineering, plastics, rubber, grinding materials, filter materials and the like.
The main components of the quartz sand are quartz and SiO2The content of the compound is more than 90-99%, wherein the impurities mainly comprise iron, aluminum, titanium, calcium, magnesium, sodium and the like. The quartz sand has high requirement on the analysis quality of the iron content due to the special requirement of industrial application of glass, ceramics and the like. The method for measuring the ferric oxide mainly comprises a phenanthroline colorimetric method, a hydrosulfate colorimetric method and a visual colorimetric method, namely a sodium sulfosalicylate colorimetric method. Although the iron content in the quartz sand can be detected by the measuring methods, the method can detect trace Fe2O3The determination of (2) has the defect of low accuracy, and the process is complicated, the consumption cost is high, and the determination of trace iron in the high-purity quartz sand is not facilitated.
In view of this, the invention provides a novel method for detecting the content of trace iron in quartz sand.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for detecting the content of trace iron in quartz sand.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for detecting the content of trace iron in quartz sand comprises the following steps:
s1, preparing a sample to be detected
Weighing siliceous sandstone, putting the siliceous sandstone into a 50ml polytetrafluoroethylene bottle resistant to high temperature and high pressure, adding 5ml concentrated hydrofluoric acid, screwing down the bottle cap, putting the bottle cap into a microwave oven, taking out the bottle cap after the siliceous sandstone is completely decomposed, and cooling the bottle cap by a water cooling device to obtain a sample to be measured;
s2 presetting Fe reagent 2
Weighing 0.6g of Fe reagent 2, putting the Fe reagent 2 into a 30ml lightproof plastic bottle, adding 5ml of ethanol and 5ml of water, and shaking until the Fe reagent 2 is completely dissolved to obtain a dissolved preset Fe reagent 2;
s3 presetting of Fe reagent 1
Measuring 10ml of Fe reagent 1, and adding 3 drops of 3% ascorbic acid to obtain a preset Fe reagent 1;
s4 color development and measurement
And (4) adding 0.2ml of the preset Fe reagent 2 into the preset Fe reagent 1 obtained in the step (S3), shaking up, adding 1ml of the sample to be detected while shaking up, and measuring by using a measuring instrument after shaking up.
More preferably: the preparation steps of the Fe reagent 2 are as follows:
5g of 1, 10-phenanthroline, 1g of ascorbic acid and 0.2g of ethylenediaminetetraacetic acid were placed in a disposable cup, ground with a marnao rod until needle crystals disappeared, and then bottled for later use to obtain Fe reagent 2.
More preferably: the preparation steps of the Fe reagent 1 are as follows:
weighing 20g of boric acid, then transferring the boric acid into a 500ml small-opening plastic bottle by using a plastic funnel, adding water to 400ml, adding 40ml of concentrated ammonia water while shaking, adding water to 500ml, covering and shaking uniformly until the boric acid is dissolved to obtain the Fe reagent 1.
More preferably: in step S1, 750 ± 5mg of siliceous sandstone with an iron content of 0.05% or less, 750 ± 5mg of siliceous sandstone with an iron content of 0.05-0.1%, and 380 ± 5mg of siliceous sandstone are weighed.
More preferably: the tester is a G3-YS tester.
More preferably: in step S1, the microwave oven selects medium-low fire, and emits microwave with intensity of 750W × 33%.
More preferably: in step S4, the sample to be measured is added and shaken up, then the mixture is stood for 5min, and then the measurement is completed within 10 min.
More preferably: in step S1, the water cooling device includes a tank body, a first cooling chamber, a second cooling chamber, and a third cooling chamber are sequentially disposed in the tank body, and partition plates are fixed between the first cooling chamber and the second cooling chamber and between the second cooling chamber and the third cooling chamber;
the cooling water is filled in the first cooling chamber, the second cooling chamber and the third cooling chamber, a water inlet pipe and a water outlet pipe are arranged on the first cooling chamber, the second cooling chamber and the third cooling chamber respectively, the temperature of the cooling water in the first cooling chamber, the second cooling chamber and the third cooling chamber is gradually reduced, and the polytetrafluoroethylene bottle filled with the material is cooled through the first cooling chamber, the second cooling chamber and the third cooling chamber in sequence.
More preferably: the water cooling device also comprises a lifting device, a horizontal moving device and a supporting device;
the lifting devices are used for driving the polytetrafluoroethylene bottles to move up and down, and the number of the lifting devices is three, and the three lifting devices are all positioned on the same side of the groove body and respectively correspond to the first cooling chamber, the second cooling chamber and the third cooling chamber; the horizontal moving device is positioned above the tank body and is used for driving the polytetrafluoroethylene bottle to sequentially pass through the first cooling chamber, the second cooling chamber and the third cooling chamber; the polytetrafluoroethylene bottle is supported on the supporting device;
the lifting device comprises a first motor, a frame body, a first screw rod and a first electromagnet, the frame body is fixed on one side of the groove body, the first screw rod is located in the frame body, the first screw rod is vertically arranged, the lower end of the first screw rod is rotatably connected with the frame body, the upper end of the first screw rod penetrates through the top of the frame body and is connected with an output shaft of the first motor, the first motor is installed on the frame body, a slotted hole is formed in one side, close to the groove body, of the frame body, the first electromagnet is sleeved on the first screw rod and is in threaded connection with the first screw rod, the first electromagnet is in up-and-down sliding fit with the frame body, the first electromagnet penetrates through the slotted hole and is in contact with the outer side of the groove body, and the first electromagnet is used for being magnetically connected with;
the horizontal moving device comprises two mounting plates, a shell, a second motor, a second electromagnet and a second screw rod, wherein the two mounting plates are respectively fixed on two opposite sides of the groove body, one mounting plate is positioned on the outer side of the first cooling chamber, the other mounting plate is positioned on the outer side of the third cooling chamber, the second screw rod is horizontally arranged, one end of the second screw rod is rotatably connected with the mounting plate, the other end of the second screw rod penetrates through the other mounting plate and is fixed with an output shaft of the second motor, the second motor is arranged on the mounting plates, the shell is fixed between the two mounting plates, the second screw rod is positioned in the shell, the bottom of the shell is provided with an opening, the second electromagnet is sleeved on the second screw rod and is in threaded connection with the second screw rod, and the second electromagnet is in horizontal sliding fit with the shell, the second electromagnet is used for being magnetically connected with the supporting device so that the polytetrafluoroethylene bottle can move along the axial direction of the second screw rod.
More preferably: the supporting device comprises a supporting plate, an iron plate, a lower connecting rod, an iron block and an upper connecting rod;
the supporting plate is used for being supported at the bottom of the polytetrafluoroethylene bottle, one end of the lower connecting rod is fixed to the supporting plate, the other end of the lower connecting rod is fixed to the iron plate, the iron plate is in contact with the inner side wall of the groove body, the first electromagnet is used for being magnetically connected with the iron plate, the upper connecting rod is located on the lower connecting rod, one end of the upper connecting rod is fixed to the iron plate, the other end of the upper connecting rod is fixed to an elastic ring, and the elastic ring is used for being sleeved on the upper portion of;
the iron block is fixed on the upper connecting rod, a groove matched with the upper connecting rod is formed in the bottom of the second electromagnet, and the second electromagnet is magnetically connected with the iron block to drive the supporting device and the polytetrafluoroethylene bottle to move horizontally.
In conclusion, the invention has the following beneficial effects: the method comprises the steps of pretreating the siliceous sandstone to discharge organic matters, volatile impurities or a small amount of carbonate, sulfide, water of combination and the like in the siliceous sandstone, preparing and presetting a color developing solution, adding a sample to be tested for color development, and finally testing by a G3-YS tester to obtain test data and realize a rapid test function. Simple process, self-preparation of color developing solution, low measurement cost, and accurate and rapid realization of trace Fe in high-purity quartz sand2O3The measurement of (1).
Drawings
FIG. 1 is a schematic structural diagram of an embodiment, which is mainly used for embodying the overall structure of a water cooling device;
FIG. 2 is a schematic top view of the embodiment, which is mainly used for showing the structure of the water cooling device;
FIG. 3 is a schematic structural diagram of the embodiment, which is mainly used for embodying the internal structure of the water cooling device;
FIG. 4 is a schematic structural diagram of an embodiment, which is mainly used for embodying a specific structure of a horizontal moving device;
FIG. 5 is a schematic structural view of the embodiment, which is mainly used for embodying the matching structure of the lifting device and the supporting device;
fig. 6 is a schematic structural diagram of the embodiment, which is mainly used for embodying the structure of the lifting device.
In the figure, 1, a trough body; 101. a first cooling chamber; 102. a second cooling chamber; 103. a third cooling chamber; 2. a water outlet pipe; 3. a water inlet pipe; 4. a lifting device; 41. a first motor; 42. a frame body; 43. a slot; 44. a first lead screw; 45. a first chute; 46. a first electromagnet; 5. a horizontal moving device; 51. mounting a plate; 52. a housing; 53. a second motor; 54. a second electromagnet; 55. a groove; 56. a second lead screw; 57. an opening; 6. a partition plate; 7. a polytetrafluoroethylene bottle; 8. a support device; 81. a support plate; 82. an iron plate; 83. a lower connecting rod; 84. an elastic ring; 85. an iron block; 86. an upper connecting rod; 9. and (6) accommodating the tank.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
In the following examples, all the raw materials used for preparation, measurement, and the like were commercially available.
Example 1: a method for detecting the content of trace iron in quartz sand comprises the following steps:
s1, preparing a sample to be detected
Weighing siliceous sandstone with iron content below 0.05% to 750 + -5 mg, placing into a high-temperature and high-pressure resistant 50ml polytetrafluoroethylene bottle 7, adding 5ml concentrated hydrofluoric acid, screwing down the bottle cap, placing into a microwave oven, taking out after siliceous sandstone is completely decomposed (about 25-30min), and cooling by a water cooling device to obtain a sample to be tested.
More preferably, the polytetrafluoroethylene bottle 7 may be a material bottle of various geometric shapes such as a conical flask and a flask.
Further preferably, the microwave oven is used for heating with medium-low fire and the emitted microwave intensity is 750W 33%.
S2 presetting Fe reagent 2
Preparing a Fe reagent 2: 5g of 1, 10-phenanthroline, 1g of ascorbic acid and 0.2g of ethylenediaminetetraacetic acid (EDTA) were placed in a disposable cup, ground with a marnastick until needle crystals disappeared, and then bottled for use to obtain Fe reagent 2. The shelf life of the Fe reagent 2 is 6 months.
Preparing a preset Fe reagent 2: weighing 0.6g of Fe reagent 2, putting the Fe reagent 2 into a 30ml lightproof plastic bottle, adding 5ml of ethanol and 5ml of water, and shaking until the Fe reagent 2 is completely dissolved to obtain the dissolved preset Fe reagent 2. Preset Fe reagent 2 for one week.
S3 presetting of Fe reagent 1
Preparing a Fe reagent 1: weighing 20g of boric acid, then transferring the boric acid into a 500ml small-opening plastic bottle by using a plastic funnel, adding water to 400ml, adding 40ml of concentrated ammonia water while shaking, adding water to 500ml, covering and shaking uniformly until the boric acid is dissolved for later use, thus obtaining the Fe reagent 1.
Further preferably, the cover needs to be closed immediately after the Fe reagent 1 is used up each time, so that the alkalinity can be prevented from changing.
Preparing a preset Fe reagent 1: 10ml of Fe reagent 1 is weighed into a plastic cup, 3 drops of 3% ascorbic acid are added, and the preset Fe reagent 1 is obtained.
S4 color development and measurement
And (4) adding 0.2ml of the preset Fe reagent 2 into the preset Fe reagent 1 obtained in the step (S3), shaking up, adding 1ml of the sample to be detected while shaking up, and measuring by using a G3-YS measuring instrument after shaking up.
Preferably, the sample to be measured is added and shaken up, then the mixture is stood for 5min, and then the measurement is finished within 10 min.
In the measurement process, 0.093% of Fe is used as a blank in water2O3The national standard of siliceous sandstone with content is used as reference. Preparing a standard sample: the siliceous sandstone is weighed to be about 1.8g, and is added with 25ml of hydrofluoric acid to be used as a reference after dissolution.
In the technical scheme, the siliceous sandstone is firstly subjected toPre-treating to discharge organic matter, volatile impurity or small amount of carbonate, sulfide, water of combination, etc. in siliceous sandstone, compounding and setting color developing liquid, adding sample to be tested for color development, and final test in G3-YS tester to obtain test data and realize fast test. Simple process, self-preparation of color developing solution, low measurement cost, and accurate and rapid realization of trace Fe in high-purity quartz sand2O3The measurement of (1).
As shown in fig. 1 to 6, in step S1, the water cooling device includes a tank body 1, a lifting device 4, a horizontal movement device 5, and a support device 8. A first cooling chamber 101, a second cooling chamber 102 and a third cooling chamber 103 are sequentially arranged in the tank body 1, and partition plates 6 are fixed between the first cooling chamber 101 and the second cooling chamber 102 and between the second cooling chamber 102 and the third cooling chamber 103, so that the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 are relatively isolated. The height of the partition plate 6 is lower than that of the side wall of the tank body 1, and cooling water is filled in the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103. The cooling water level is always located below the top surface of the partition 6 to prevent the cooling water in the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 from communicating with each other. The first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 are respectively provided with a water inlet pipe 3 and a water outlet pipe 2, the water inlet pipe 3 is positioned on one side of the upper parts of the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103, and the water outlet pipe 2 is positioned on one side of the lower parts of the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103. The water inlet pipe 3 and the water outlet pipe 2 are both positioned at the same side of the tank body 1.
Further preferably, the cooling water is circulating water, and the circulating water continuously enters and exits through the water inlet pipe 3 and the water outlet pipe 2, so that the temperature of the cooling water does not change greatly in the material cooling process.
As shown in fig. 1 to 6, the temperature of the cooling water in the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 is gradually decreased, and the polytetrafluoroethylene bottle 7 containing the material is cooled in order through the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103. Specifically, the temperature of the cooling water in the first cooling chamber 101 is 40 ± 2 ℃, the temperature of the cooling water in the second cooling chamber 102 is 20 ± 2 ℃, and the temperature of the cooling water in the third cooling chamber 103 is 5 ± 2 ℃. The cooling time of the polytetrafluoroethylene bottle 7 in the first cooling chamber 101 is 5min, the cooling time in the second cooling chamber 102 is 3min, and the cooling time in the third cooling chamber 103 is 1-2 min.
In the above technical solution, if the material bottle is overheated, the material bottle may crack or even explode due to the drastic change of the temperature. Therefore, the invention adopts a step-type water cooling mode with gradually lowered temperature to gradually cool the materials in the polytetrafluoroethylene bottle 7. Because the material bottle used by the invention is the polytetrafluoroethylene bottle 7, even though the polytetrafluoroethylene bottle 7 is suddenly added with the super-cooling water under the condition of overheating, the polytetrafluoroethylene bottle 7 cannot be burst or cracked, but the aging of the polytetrafluoroethylene bottle 7 is accelerated, and the service life of the polytetrafluoroethylene bottle 7 is influenced. Therefore, in order to prevent the material bottles from aging, cracking, exploding and the like, the invention designs the water cooling device which is suitable for the material bottles made of various materials and has wide application range.
As shown in fig. 1 to 6, the lifting device 4 is used to move the teflon bottle 7 up and down so that the teflon bottle 7 is immersed in or separated from the cooling water. The lifting devices 4 are three, and the three lifting devices 4 are all located on the same side of the tank body 1 and correspond to the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 respectively. The lifting device 4 and the water inlet pipe 3 are respectively positioned at two opposite sides of the tank body 1. The lifting device 4 includes a first motor 41, a frame 42, a first lead screw 44, and a first electromagnet 46. The frame body 42 is fixed on one side of the tank body 1, the first screw rod 44 is positioned in the frame body 42, the first screw rod 44 is vertically arranged, the lower end of the first screw rod is rotatably connected with the frame body 42, and the upper end of the first screw rod passes through the top of the frame body 42 and is connected with an output shaft of the first motor 41. The first motor 41 is mounted on the frame 42. The frame 42 is provided with a slot 43 on one side close to the tank 1, the slot 43 is located on one side of the tank 1, and the first electromagnet 46 is sleeved on the first screw rod 44 and is in threaded connection with the first screw rod 44. The first electromagnet 46 is in up-and-down sliding fit with the frame body 42, first sliding blocks are fixed on two sides of the first electromagnet 46, and a first sliding groove 45 matched with the first sliding blocks is formed in the side wall of the frame body 42. The first sliding groove 45 is vertical, and the first sliding block is embedded in the first sliding groove 45 and is in sliding fit with the first sliding groove 45. The first electromagnet 46 penetrates through the slotted hole 43 and contacts with the outer side of the groove body 1, and the first electromagnet 46 is used for being magnetically connected with the supporting device 8 so as to enable the polytetrafluoroethylene bottle 7 to move up and down. The teflon bottle 7 is supported on a support means 8.
As shown in fig. 1-6, the horizontal moving device 5 is located at one side above the tank body 1 and is used for driving the teflon bottle 7 to pass through the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 in sequence. The horizontal moving device 5 includes a mounting plate 51, a housing 52, a second motor 53, a second electromagnet 54, and a second lead screw 56. The two mounting plates 51 are provided, the two mounting plates 51 are respectively fixed on two opposite sides of the tank body 1, one mounting plate 51 is located outside the first cooling chamber 101, and the other mounting plate 51 is located outside the third cooling chamber 103. The second screw rod 56 is horizontally arranged, one end of the second screw rod is rotatably connected with the mounting plate 51, the other end of the second screw rod penetrates through the other mounting plate 51 and is fixed with an output shaft of the second motor 53, and the second motor 53 is mounted on the mounting plate 51. The housing 52 is fixed between the two mounting plates 51, the second lead screw 56 is located in the housing 52, and the bottom of the housing 52 is provided with an opening 57. The second electromagnet 54 is sleeved on the second screw rod 56 and is in threaded connection with the second screw rod 56, and the second electromagnet 54 is in horizontal sliding fit with the shell 52. Specifically, the second sliding block is fixed on two sides of the second electromagnet 54, and the inner wall of the housing 52 is provided with a second sliding groove matched with the second sliding block. The second sliding groove is horizontal, and the second sliding block is embedded in the second sliding groove and is in sliding fit with the second sliding groove. The second electromagnet 54 is used for magnetically connecting with the supporting device 8 so as to move the polytetrafluoroethylene bottle 7 along the axial direction of the second screw rod 56.
As shown in fig. 1 to 6, the supporting device 8 includes a supporting plate 81, an iron plate 82, a lower connecting rod 83, an iron block 85, and an upper connecting rod 86. The supporting plate 81 is used for supporting the bottom of the polytetrafluoroethylene bottle 7, one end of the lower connecting rod 83 is fixed with the supporting plate 81, and the other end of the lower connecting rod is fixed with the lower part of the iron plate 82. The iron plate 82 is contacted with the inner side wall of the tank body 1, the upper connecting rod 86 is positioned on the lower connecting rod 83, one end of the upper connecting rod is fixed on the iron plate 82, the other end of the upper connecting rod is fixed with an elastic ring 84, and the elastic ring 84 is used for being sleeved on the upper part of the polytetrafluoroethylene bottle 7 so as to prevent the polytetrafluoroethylene bottle 7 from toppling over. The iron block 85 is fixed on the upper connecting rod 86, the bottom of the second electromagnet 54 is provided with a groove 55 matched with the upper connecting rod 86, and the iron block 85 is inserted into the groove 55. The second electromagnet 54 is used for being magnetically connected with the iron block 85 so as to drive the supporting device 8 and the polytetrafluoroethylene bottle 7 to horizontally move. The first electromagnet 46 is used for being magnetically connected with the iron plate 82 so as to drive the supporting device 8 and the polytetrafluoroethylene bottle 7 to move up and down. The bottom in the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103 is provided with an accommodating groove 9 matched with the lower connecting rod 83, and when the supporting plate 81 contacts with the bottoms of the first cooling chamber 101, the second cooling chamber 102 and the third cooling chamber 103, the bottom of the lower connecting rod 83 is positioned in the accommodating groove 9.
In the above technical solution, when the teflon bottle 7 is transferred from the first cooling chamber 101 to the second cooling chamber 102, or transferred from the second cooling chamber 102 to the third cooling chamber 103, the first electromagnet 46 is energized to magnetically connect the first electromagnet 46 with the iron plate 82, and then the first motor 41 is started to rotate the first lead screw 44 in the frame 42, because the first electromagnet 46 is sleeved on the first lead screw 44 and is in threaded connection with the first lead screw 44, and the first electromagnet 46 is in up-and-down sliding fit with the frame 42, when the first lead screw 44 rotates, the first electromagnet 46 drives the iron plate 82, the support plate 81, and the teflon bottle 7 to move upwards until the iron block 85 is inserted into the groove 55. After the iron block 85 is inserted into the groove 55, the second electromagnet 54 is powered on, the first electromagnet 46 is powered off, the first motor 41 stops running, then the second motor 53 is started, so that the supporting device 8 and the polytetrafluoroethylene bottle 7 integrally and horizontally move to the position above the second cooling chamber 102 or the third cooling chamber 103, and then the supporting device 8 and the polytetrafluoroethylene bottle 7 are moved into the second cooling chamber 102 or the third cooling chamber 103 through the lifting device 4 corresponding to the second cooling chamber 102 or the third cooling chamber 103.
Example 2: the method for detecting the content of trace iron in quartz sand is different from that in example 1 in that 380 +/-5 mg of siliceous sandstone is weighed, and the content of iron is 0.05-0.1%.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that several improvements and modifications without departing from the principle of the present invention will occur to those skilled in the art, and such improvements and modifications should also be construed as within the scope of the present invention.
Claims (10)
1. A method for detecting the content of trace iron in quartz sand is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing a sample to be detected
Weighing siliceous sandstone, putting the siliceous sandstone into a 50ml polytetrafluoroethylene bottle (7) resistant to high temperature and high pressure, adding 5ml concentrated hydrofluoric acid, screwing a bottle cap, putting the bottle cap into a microwave oven, taking out the siliceous sandstone after the siliceous sandstone is completely decomposed, and cooling the siliceous sandstone by a water cooling device to obtain a sample to be measured;
s2 presetting Fe reagent 2
Weighing 0.6g of Fe reagent 2, putting the Fe reagent 2 into a 30ml lightproof plastic bottle, adding 5ml of ethanol and 5ml of water, and shaking until the Fe reagent 2 is completely dissolved to obtain a dissolved preset Fe reagent 2;
s3 presetting of Fe reagent 1
Measuring 10ml of Fe reagent 1, and adding 3 drops of 3% ascorbic acid to obtain a preset Fe reagent 1;
s4 color development and measurement
And (4) adding 0.2ml of the preset Fe reagent 2 into the preset Fe reagent 1 obtained in the step (S3), shaking up, adding 1ml of the sample to be detected while shaking up, and measuring by using a measuring instrument after shaking up.
2. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: the preparation steps of the Fe reagent 2 are as follows:
5g of 1, 10-phenanthroline, 1g of ascorbic acid and 0.2g of ethylenediaminetetraacetic acid were placed in a disposable cup, ground with a marnao rod until needle crystals disappeared, and then bottled for later use to obtain Fe reagent 2.
3. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: the preparation steps of the Fe reagent 1 are as follows:
weighing 20g of boric acid, then transferring the boric acid into a 500ml small-opening plastic bottle by using a plastic funnel, adding water to 400ml, adding 40ml of concentrated ammonia water while shaking, adding water to 500ml, covering and shaking uniformly until the boric acid is dissolved to obtain the Fe reagent 1.
4. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: in step S1, 750 ± 5mg of siliceous sandstone with an iron content of 0.05% or less, 750 ± 5mg of siliceous sandstone with an iron content of 0.05-0.1%, and 380 ± 5mg of siliceous sandstone are weighed.
5. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: the tester is a G3-YS tester.
6. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: in step S1, the microwave oven selects medium-low fire, and emits microwave with intensity of 750W × 33%.
7. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: in step S4, the sample to be measured is added and shaken up, then the mixture is stood for 5min, and then the measurement is completed within 10 min.
8. The method for detecting the content of trace iron in quartz sand according to claim 1, wherein the method comprises the following steps: in step S1, the water cooling device includes a tank body (1), a first cooling chamber (101), a second cooling chamber (102), and a third cooling chamber (103) are sequentially disposed in the tank body (1), and partition plates (6) are fixed between the first cooling chamber (101) and the second cooling chamber (102) and between the second cooling chamber (102) and the third cooling chamber (103);
cooling water is filled in the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103), a water inlet pipe (3) and a water outlet pipe (2) are respectively arranged on the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103), the temperature of the cooling water in the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103) is gradually reduced, and the polytetrafluoroethylene bottle (7) filled with materials is sequentially cooled through the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103).
9. The method for detecting the content of trace iron in quartz sand according to claim 8, wherein the method comprises the following steps: the water cooling device also comprises a lifting device (4), a horizontal moving device (5) and a supporting device (8);
the lifting devices (4) are used for driving the polytetrafluoroethylene bottle (7) to move up and down, the number of the lifting devices (4) is three, and the three lifting devices (4) are located on the same side of the tank body (1) and respectively correspond to the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103); the horizontal moving device (5) is positioned above the tank body (1) and is used for driving the polytetrafluoroethylene bottle (7) to sequentially pass through the first cooling chamber (101), the second cooling chamber (102) and the third cooling chamber (103); the polytetrafluoroethylene bottle (7) is supported on the supporting device (8);
the lifting device (4) comprises a first motor (41), a frame body (42), a first screw rod (44) and a first electromagnet (46), the frame body (42) is fixed on one side of the tank body (1), the first screw rod (44) is located in the frame body (42), the first screw rod (44) is vertically arranged, the lower end of the first screw rod is rotatably connected with the frame body (42), the upper end of the first screw rod penetrates through the top of the frame body (42) and is connected with an output shaft of the first motor (41), the first motor (41) is installed on the frame body (42), a slotted hole (43) is formed in one side, close to the tank body (1), of the frame body (42), the first electromagnet (46) is sleeved on the first screw rod (44) and is in threaded connection with the first screw rod (44), the first electromagnet (46) is in up-down sliding fit with the frame body (42), the first electromagnet (46) penetrates through the slotted hole (43) and is in contact with the outer side of the tank body (1), the first electromagnet (46) is magnetically connected with the supporting device (8) so as to move the polytetrafluoroethylene bottle (7) up and down;
horizontal migration device (5) includes mounting panel (51), shell (52), second motor (53), second electro-magnet (54) and second lead screw (56), mounting panel (51) are provided with two, two mounting panel (51) are fixed respectively the relative both sides of cell body (1) and one of them mounting panel (51) are located the first cooling chamber (101) outside, another mounting panel (51) are located the third cooling chamber (103) outside, second lead screw (56) are horizontal setting and one end with mounting panel (51) rotate the connection, the other end pass another mounting panel (51) and with second motor (53) output shaft is fixed, second motor (53) are installed on mounting panel (51), shell (52) are fixed two between mounting panel (51), second lead screw (56) are located in shell (52), an opening (57) is formed in the bottom of the shell (52), the second electromagnet (54) is sleeved on the second screw rod (56) and is in threaded connection with the second screw rod (56), the second electromagnet (54) is in horizontal sliding fit with the shell (52), and the second electromagnet (54) is used for being in magnetic connection with the supporting device (8) so that the polytetrafluoroethylene bottle (7) can move along the axial direction of the second screw rod (56).
10. The method for detecting the content of trace iron in quartz sand according to claim 9, wherein the method comprises the following steps: the supporting device (8) comprises a supporting plate (81), an iron plate (82), a lower connecting rod (83), an iron block (85) and an upper connecting rod (86);
the supporting plate (81) is used for being supported at the bottom of the polytetrafluoroethylene bottle (7), one end of the lower connecting rod (83) is fixed to the supporting plate (81), the other end of the lower connecting rod is fixed to the iron plate (82), the iron plate (82) is in contact with the inner side wall of the groove body (1), the first electromagnet (46) is used for being magnetically connected with the iron plate (82), the upper connecting rod (86) is located on the lower connecting rod (83), one end of the upper connecting rod is fixed to the iron plate (82), the other end of the upper connecting rod is fixed to the elastic ring (84), and the elastic ring (84) is used for being sleeved on the upper portion of the polytetrafluoroethylene bottle (7);
the iron block (85) is fixed on the upper connecting rod (86), a groove (55) matched with the upper connecting rod (86) is formed in the bottom of the second electromagnet (54), and the second electromagnet (54) is magnetically connected with the iron block (85) to drive the supporting device (8) and the polytetrafluoroethylene bottle (7) to move horizontally.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010819422.7A CN112014386A (en) | 2020-08-14 | 2020-08-14 | Method for detecting content of trace iron in quartz sand |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010819422.7A CN112014386A (en) | 2020-08-14 | 2020-08-14 | Method for detecting content of trace iron in quartz sand |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112014386A true CN112014386A (en) | 2020-12-01 |
Family
ID=73504499
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010819422.7A Pending CN112014386A (en) | 2020-08-14 | 2020-08-14 | Method for detecting content of trace iron in quartz sand |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112014386A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590108A (en) * | 2012-01-06 | 2012-07-18 | 安徽省石英砂及制品质量监督检验中心 | Method for quickly and efficiently detecting content of trace elements in quartz sand through microwave digestion |
| CN103604803A (en) * | 2013-11-11 | 2014-02-26 | 深圳大学 | Method for rapidly detecting content of iron ion in red wine |
| CN207290672U (en) * | 2017-06-28 | 2018-05-01 | 广东冠盛塑胶有限公司 | A kind of improved pvc film cooling apparatus |
| CN108607948A (en) * | 2016-12-13 | 2018-10-02 | 重庆市道诚机械有限公司 | The gradual gradient cooling cooling device of punching block |
-
2020
- 2020-08-14 CN CN202010819422.7A patent/CN112014386A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590108A (en) * | 2012-01-06 | 2012-07-18 | 安徽省石英砂及制品质量监督检验中心 | Method for quickly and efficiently detecting content of trace elements in quartz sand through microwave digestion |
| CN103604803A (en) * | 2013-11-11 | 2014-02-26 | 深圳大学 | Method for rapidly detecting content of iron ion in red wine |
| CN108607948A (en) * | 2016-12-13 | 2018-10-02 | 重庆市道诚机械有限公司 | The gradual gradient cooling cooling device of punching block |
| CN207290672U (en) * | 2017-06-28 | 2018-05-01 | 广东冠盛塑胶有限公司 | A kind of improved pvc film cooling apparatus |
Non-Patent Citations (1)
| Title |
|---|
| 上海市化工轻工供应公司 上海化工采购供应站 技术室编: "《化工商品检验方法》", 31 October 1988, 化学工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hydes | Aluminum in seawater: Control by inorganic processes | |
| CN206270237U (en) | A kind of multifunctional sample reaction detection room for the analysis of QPQ technology bases salt component | |
| CN111982951A (en) | Method for processing sample and determining element content | |
| CN106053462B (en) | The measuring method of Determination of Trace Thallium in a kind of water | |
| CN112014386A (en) | Method for detecting content of trace iron in quartz sand | |
| Osugi et al. | Effect of oxidation state of iron ions on the viscosity of alkali silicate melts | |
| CN103822850A (en) | Method for determination of content of calcium metal in calcium-series cored wires | |
| CN113624794A (en) | Test device and method for evaluating molten iron corrosion resistance of blast furnace carbon brick | |
| CN113295760A (en) | Method for simultaneously measuring low contents of lanthanum, cerium, praseodymium, neodymium, samarium and barium in furnace slag and mold powder | |
| CN111650194A (en) | Method for determining phosphorus content in iron ore by bismuth-phosphorus-molybdenum blue | |
| CN110618020A (en) | Method for rapidly digesting heavy metal soil sample | |
| CN110672577A (en) | Method for measuring selenium content in rice | |
| CN212693419U (en) | Water cooling device for measuring content of trace iron in quartz sand | |
| CN104062285A (en) | Determination method for contents of calcium, aluminum and silicon elements in solid surface materials | |
| CN111443056B (en) | Method for measuring mercury content in copper concentrate | |
| CN105044074B (en) | A kind of method that utilization silicon substrate chemical sensing material detects water pollutant concentration | |
| CN111323280A (en) | Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass | |
| CN113218934A (en) | Detection method for rapidly determining content of yttrium in steel by utilizing full-spectrum spark direct-reading spectrometry | |
| CN220170689U (en) | A preceding stage ashing digestion device for organic fertilizer phosphorus/potassium content measurement | |
| CN87212029U (en) | Constant-temperature type automatic calorimeter | |
| CN114199667B (en) | Pretreatment method of azodiisobutyronitrile and determination method of trace element content | |
| CN220961163U (en) | Corrosion-resistant device for measuring substrate glass kiln electric melting high-zirconium brick | |
| CN118443708A (en) | Method for measuring calcium fluoride in dolomite-containing ore | |
| CN210487653U (en) | Device for preparing spectral analysis sample | |
| CN117214075A (en) | Device and method for measuring corrosion resistance of substrate glass kiln electric smelting high-zirconium brick |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201201 |
|
| RJ01 | Rejection of invention patent application after publication |