CN115711857B - Residual detection experimental device and detection method for lead ion standard solution - Google Patents
Residual detection experimental device and detection method for lead ion standard solution Download PDFInfo
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- CN115711857B CN115711857B CN202310016920.1A CN202310016920A CN115711857B CN 115711857 B CN115711857 B CN 115711857B CN 202310016920 A CN202310016920 A CN 202310016920A CN 115711857 B CN115711857 B CN 115711857B
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Abstract
The invention relates to the technical field of metal ion detection devices, in particular to a residual detection experimental device and a detection method of a lead ion standard solution; the invention relates to a residual detection experimental device for a lead ion standard solution, which comprises a pulverizer, a baking furnace, an ashing furnace and a spectrometer; the ashing furnace in this embodiment may be a muffle furnace; a transfer mechanism is arranged on the ashing furnace; the transfer mechanism can transfer the support in the ashing furnace and the sample crucible into the furnace door, so that the temperature reduction rate of the sample crucible is reduced, and the sample crucible is prevented from being fried; according to the invention, the transfer mechanism is arranged on the furnace door, so that when ashing is carried out on a plurality of different types of samples, the bracket and the sample crucible in the furnace body are moved to the transfer groove through the sampling block and then are moved out of the furnace from the transfer groove, the temperature reduction rate of the sample crucible is slowed down, and the problem that the sample crucible is exploded due to the sudden temperature drop is solved.
Description
Technical Field
The invention relates to the technical field of metal ion detection devices, in particular to a residual detection experimental device and a detection method for a lead ion standard solution.
Background
Lead and lead compounds are one of 17 chemical substances seriously jeopardizing human life and natural environment, and the existence of excessive lead in human body can lead to disorder of nerve and regeneration system, hypoevolutism, hypohemoglobin and anemia and hypertension; therefore, people detect the residues of lead ions in food or living environment so as to ensure the food safety or environmental safety of people;
when detecting the residue of lead ions in food, firstly sampling the food, then carrying out dry digestion on the sample to enable lead elements in the sample to be in an ionic state, and then detecting the sample by using a spectrum instrument;
during dry digestion, firstly taking a quantitative sample, drying the sample, continuously heating to carbonize the sample, then placing the sample into a heating furnace to heat so as to ashe the carbonized sample, and then preparing the ashed sample into a sample solution;
when taking out the sample crucible from the ashing furnace, the sample crucible is easy to burst due to temperature dip, so that the sample is damaged, if the sample crucible is placed at the furnace mouth of the furnace body for cooling, a large amount of heat in the furnace can be diffused from the furnace mouth, so that the temperature of the ashed sample and the sample crucible in the furnace body is uneven, the ashing effect is influenced, and the problem of energy waste is caused, so that the limitation is caused.
Therefore, we propose a residual detection experimental device and a detection method for lead ion standard solution.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a residual detection experimental device and a detection method for a lead ion standard solution, overcomes the defects of the prior art and aims at solving the problems in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions: a residual detection experimental device for lead ion standard solution comprises
Pulverizer, roaster, ashing furnace and spectrometer; the ashing furnace in this embodiment may be a muffle furnace;
the ashing furnace comprises a furnace body and a furnace door; a chute is formed in the furnace body; the sample is clamped in the chute through a bracket;
a transfer mechanism is arranged on the ashing furnace; the transfer mechanism can transfer the inner support of the ashing furnace and the sample crucible into the furnace door, so that the temperature reduction rate of the sample crucible is reduced, and the sample crucible is prevented from being fried.
Preferably, the transfer mechanism comprises a transfer groove, a take-out block and a sealing block; the transfer groove is formed in the furnace door; the furnace door is uniformly provided with sliding grooves; the taking-out block is connected in the sliding groove in a sliding way; one end of the taking-out block, which is close to the inside of the furnace body, is arranged in a concave shape and can be clamped with the bracket, and one concave end of the taking-out block is rotationally connected with a clamping rod; the clamping rod is obliquely arranged; the sealing block is rotationally connected to the end face of the furnace door, which is close to the furnace body, and can plug the transfer groove;
a driving unit is arranged in the furnace door and used for driving the sealing block to rotate; the extraction block is made of heat-insulating materials; in this embodiment, the take-out block is made of a ceramic insulating material.
Preferably, the take-out block is provided with a rope hole; a steel wire rope is arranged in the rope hole; one end of the steel wire rope is fixedly connected with the clamping rod, and the other end of the steel wire rope is exposed out of the taking-out block.
The transfer mechanism is arranged on the furnace door, so that when ashing is carried out on a plurality of different types of samples, the bracket and the sample crucible in the furnace body are moved to the transfer tank through the sampling block and then are moved out of the furnace from the transfer tank, the temperature reduction rate of the sample crucible is slowed down, the problem that the sample crucible is fried due to the sudden temperature drop is solved, and meanwhile, different types of samples are borne by different brackets, so that when the ashed samples are taken out, the furnace door is not required to be opened, heat in the furnace body is scattered unevenly, and the ashing effect of the other types of samples is affected; the ashing completion times of different types of samples can be staggered, and the ashed samples can be detected when the rest samples are ashed, so that the efficiency is improved.
Preferably, a vertical groove is formed in one end, close to the bracket, of the extraction block in the furnace body.
Through placing support and sample crucible in the perpendicular inslot on taking out the piece to when taking out the piece and taking support and sample crucible reentry in the furnace body, take out the piece and prevent support and closed piece contact, thereby make support and sample crucible shake, the condition that the sample was shaken out appears.
Preferably, the wall of the sliding groove is rotatably connected with a plugging plate; the driving unit is also arranged below the plugging plate.
Preferably, the driving unit comprises a balancing weight, a cavity, a connecting rope and a through hole; the cavity is arranged in the furnace door and is positioned below the transfer groove; the balancing weight is positioned in the cavity; the through hole is positioned at the upper end of the cavity and is communicated with the cavity; one end of the connecting rope is fixedly connected with the balancing weight; the connecting rope below the sealing block is fixedly connected with the sealing block; a turntable is rotationally connected below the plugging plate, and the connecting rope below the plugging plate is fixedly connected with the outer side surface of the turntable; in this embodiment, the connecting rope is made of steel wire rope.
The gravity driving sealing block and the sealing plate of the balancing weight in the driving unit return to the original positions, and meanwhile, the connecting rope is made of a steel wire rope and can resist high temperature, so that compared with the torsion spring and other components, the sealing block and the sealing plate can be used for a long time in the high-temperature environment of the furnace mouth of the furnace body, the situation that the similar torsion spring fails due to the fact that the torsion spring is in the high-temperature environment for a long time can not occur, and the using effect of the sealing block and the sealing plate is guaranteed.
Preferably, the number of the sealing blocks is the same as that of the taking-out blocks, and the positions of the sealing blocks correspond to those of the taking-out blocks; the size of the cross section of the closing block is the same as that of the cross section of the taking-out block.
Preferably, the taking-out block is formed by rotationally connecting a first block and a second block; the first block is far away from the furnace body and can rotate downwards; the furnace door is provided with a clamping groove.
The method is suitable for the experimental device for detecting the residue of the lead ion standard solution, and comprises the following steps:
s1, placing grain crops into a pulverizer to pulverize, then placing quantitative pulverized grain crop powder into a sample crucible, placing the sample crucible on a baking furnace to bake with small fire to carbonize the sample, placing the sample crucible into a bracket, and then placing the sample crucible and the bracket into an ashing furnace to ash;
s2, after ashing the sample, moving the bracket and the sample crucible to a transfer groove through a taking-out block, so that the bracket and the sample crucible are cooled in an environment that the transfer groove is higher than room temperature, and then taking out the taking-out block together with the bracket and the sample crucible from the sliding groove;
s3, placing the sample crucible in a room temperature environment for cooling, and adding GR nitric acid into the sample crucible after the sample crucible is cooled to room temperature, wherein the ratio of the GR nitric acid to the sample is 1ml:1g, placing the sample crucible on a heating furnace for evaporating, and adding nitric acid solution and water, wherein the ratio of the nitric acid solution to the water to the sample is 1ML1% nitric acid solution: 3ML water: 1g of sample is placed on a heating furnace again and heated to near boiling by small fire, so that sample solution is obtained; and then placing the sample solution and an equivalent lead ion standard solution into a spectrometer for detection, and calculating the content of lead ions in the sample solution.
The invention has the beneficial effects that:
1. according to the invention, the transfer mechanism is arranged on the furnace door, so that when ashing is carried out on a plurality of different types of samples, the bracket and the sample crucible in the furnace body are moved to the transfer tank through the sampling block and then are moved out of the furnace from the transfer tank, the temperature reduction rate of the sample crucible is slowed down, the problem that the sample crucible is fried due to the sudden temperature drop is solved, and meanwhile, different types of samples are borne by different brackets, so that when the ashed samples are taken out, the furnace door is not required to be opened, heat in the furnace body is scattered unevenly, and the ashing effect of the other types of samples is affected; the ashing completion times of different types of samples can be staggered, and the ashed samples can be detected when the rest samples are ashed, so that the efficiency is improved.
2. According to the invention, the bracket and the sample crucible are placed in the vertical groove on the taking-out block, so that when the taking-out block brings the bracket and the sample crucible into the furnace body again, the taking-out block prevents the bracket from contacting with the sealing block, and the bracket and the sample crucible shake, so that the situation that the sample is shaken out occurs.
3. According to the invention, the sealing block and the sealing plate are driven to return to the original positions by the gravity of the balancing weight in the driving unit, and meanwhile, the connecting rope is made of the steel wire rope, so that the sealing block and the sealing plate can resist high temperature, and compared with the torsion spring and other components, the sealing block and the sealing plate can be used for a long time in the high-temperature environment of the furnace mouth of the furnace body, and the condition that the similar torsion spring fails due to the long-time high-temperature environment can not occur, so that the use effect of the sealing block and the sealing plate is ensured.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is an enlarged view of FIG. 1 at A;
FIG. 3 is a cross-sectional view of the oven body and oven door of the present invention;
FIG. 4 is an enlarged view at B in FIG. 3;
FIG. 5 is a cross-sectional view of the oven door, closing block and block one from view at C-C in FIG. 3;
FIG. 6 is a cross-sectional view of the oven door, the blanking panel and the first block from the view at D-D in FIG. 3;
fig. 7 is a diagram showing the positional relationship between the first block and the bracket after the first block is engaged with the bracket.
In the figure: 1. a pulverizer; 2. baking oven; 3. an ashing furnace; 7. a spectrometer; 31. a furnace body; 32. a furnace door; 33. a bracket; 34. a chute; 4. a transfer mechanism; 41. a transfer tank; 42. taking out the block; 43. a closing block; 44. a sliding groove; 45. a clamping rod; 46. rope holes; 47. a wire rope; 48. a vertical groove; 49. a plugging plate; 5. a driving unit; 51. balancing weight; 52. a connecting rope; 53. a turntable; 54. a cavity; 55. a through hole; 61. a first block; 62. a second block; 63. and a clamping groove.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
referring to fig. 1 of the specification, a residual detection experiment device for lead ion standard solution comprises
A pulverizer 1, a baking furnace 2, an ashing furnace 3 and a spectrometer 7; the ashing furnace 3 in this embodiment may be a muffle furnace;
the ashing furnace 3 includes a furnace body 31 and a furnace door 32; a chute 34 is arranged in the furnace body 31; the sample is clamped in the chute 34 through the bracket 33;
the ashing furnace 3 is provided with a transfer mechanism 4; the transfer mechanism 4 can transfer the bracket 33 in the ashing furnace 3 and the sample crucible into the furnace door 32, so that the temperature reduction rate of the sample crucible is reduced, and the sample crucible is prevented from being fried;
referring to fig. 3 of the drawings, in the present embodiment, the transfer mechanism 4 includes a transfer tank 41, a take-out block 42, and a closing block 43; the transfer groove 41 is arranged in the furnace door 32; the furnace door 32 is uniformly provided with sliding grooves 44; the extraction block 42 is slidably coupled within the slide channel 44; one end of the withdrawing block 42, which is close to the inside of the furnace body 31, is provided with a concave shape and can be engaged with the bracket 33, and one concave end of the withdrawing block 42 is rotationally connected with a clamping rod 45; the clamping rod 45 is obliquely arranged; the closing block 43 is rotatably connected to the end surface of the furnace door 32 close to the furnace body 31, and the closing block 43 can block the transfer groove 41;
a driving unit 5 is arranged in the furnace door 32 and is used for driving the closing block 43 to rotate; the take-out block 42 is made of a heat insulating material; in this embodiment, the take-out block 42 is made of a ceramic insulating material;
referring to fig. 5 of the drawings, in this embodiment, the take-out block 42 is provided with a rope hole 46; a steel wire rope 47 is arranged in the rope hole 46; one end of the steel wire rope 47 is fixedly connected with the clamping rod 45, and the other end of the steel wire rope is exposed out of the taking-out block 42;
when a worker performs lead ion residue detection on grain crops, firstly, sampling, putting the grain crops to be detected into a grinder 1 for grinding, then taking quantitative ground grain crop powder (for example, 5 g) into a sample crucible, putting the sample crucible into a baking oven 2 for baking with small fire, baking the moisture of the sample, continuously baking to carbonize the sample, putting the sample crucible into a bracket 33, then putting the sample crucible and the bracket 33 into an ashing oven 3, setting the temperature to 750 ℃ for about three hours, wherein different sample ashing times are different, taking out the sample crucible after sample ashing is completed, cooling the sample crucible, and adding GR nitric acid into the sample crucible, wherein the ratio of GR nitric acid to the sample is 1ml:1g, then evaporating the sample crucible on a heating furnace, and adding 1ML of 1% nitric acid solution and 3ML of water after the sample crucible is cooled, wherein the ratio of the nitric acid solution and the water to the sample is 1ML of 1% nitric acid solution: 3ML water: 1g of sample is placed on a heating furnace again and heated to near boiling by small fire, so that sample solution is obtained;
and then taking the lead ion standard solution with the same quantity, simultaneously placing the standard solution and the sample solution into a spectrometer 7 for detection, respectively detecting the mass concentration of the lead ions in the sample solution and the mass concentration of the lead ions in the standard solution, and then according to a formula, wherein:
x-the content of lead ions in milligrams per kilogram or milligrams per liter (mg/kg or mg/L) of the sample;
p-mass concentration of lead ions in the sample solution in micrograms per liter (ug/L);
p0-mass concentration of lead ions in standard solution in micrograms per liter (ug/L);
v-constant volume of sample digest in milliliters (mL);
m—sample weight or removal volume in grams or milliliters (g or mL);
1000-conversion coefficient;
when the lead content is more than or equal to 1.00mg/kg (or mg/L), the calculated result keeps three valid figures; when the lead content is less than 1.00mg/kg (or mg/L), the calculated result keeps three significant digits;
in this embodiment, the temperature in the transfer tank 41 is lower than the temperature in the furnace body 31 due to the sealing of the sealing block 43 in the transfer tank 41; in this embodiment, when a worker needs to detect a plurality of different types of samples, a sample crucible containing the different types of samples is placed in different supports 33, then the plurality of supports 33 are placed in the ashing furnace 3, the furnace door 32 is closed for ashing, and the positions of the supports 33 correspond to the positions of the take-out blocks 42 on the furnace door 32; different types of samples have different ashing times because of different oil and protein contents; when ashing of the sample requiring less ashing time is completed, the worker pushes the corresponding withdrawing block 42, so that the withdrawing block 42 moves in the sliding groove 44 towards the direction approaching the sample, the withdrawing block 42 pushes the closing block 43 to rotate, the blocking plate 49 rotates, one blocked end of the transit groove 41 is exposed, then the withdrawing block 42 continues to move forwards until one concave end of the withdrawing block 42 contacts with the bracket 33 where the ashed sample is located, the clamping rod 45 is jacked by the jacking block on the bracket 33, then the clamping rod 45 is clamped on the other side of the jacking block after passing over the jacking block, so that the withdrawing block 42 clamps the bracket 33, then the worker pulls the withdrawing block 42 backwards, so that the withdrawing block 42 moves towards the furnace door 32 with the bracket 33 in the furnace body 31 until moving into the transit groove 41, and at this time, the closing block 43 does not support the withdrawing block 42, so as to block the notch of the transit groove 41 again under the action of the driving unit 5; after the temperature of the support 33 and the sample crucible in the transfer tank 41 is reduced, the worker pulls the take-out block 42 outwards again to separate the take-out block 42 from the sliding tank 44, then the worker pulls the steel wire rope 47 on the take-out block 42, so that the steel wire rope 47 pulls the clamping rod 45 to rotate to separate the clamping rod 45 from the top block on the support 33, at the moment, the worker uses pliers or other tools to take the support 33 off the take-out block 42, and then the worker inserts the take-out block 42 into the sliding tank 44;
in the embodiment, by arranging the transfer groove 41, the sample crucible is moved to the transfer groove 41 when the sample crucible is taken out, and cooling is performed; the staff can take out the sample crucible after sample ashing in the furnace body 31 through the taking-out block 42, and other samples and the sample crucible are still in the furnace body 31, so that the staff can take out the ashed samples under the condition that the ashing of other samples is not affected, and therefore, the staff can ash a plurality of different types of samples simultaneously, the ashing completion time of the samples is staggered, and the ashed samples are detected when the other samples are ashed, so that the efficiency is improved;
compared with the mode of directly opening the furnace door 32 and taking out the sample crucible, in the embodiment, the temperature of the sample crucible is higher than the room temperature because of the transfer tank 41, so that the temperature of the sample crucible is cooled from the inside of the furnace body 31 to the transfer tank 41 and from the transfer tank 41 to the outside of the furnace, and the problem that the sample crucible is exploded due to the sudden temperature drop is further reduced; meanwhile, compared with the embodiment of opening the furnace door 32 and placing the sample crucible at the furnace mouth of the furnace body 31 for cooling, the embodiment does not cause a large amount of heat in the furnace to diffuse from the furnace mouth, so that the temperature of the sample and the sample crucible still ashed in the furnace body 31 is uneven, and the problem of affecting the ashing effect is solved;
according to the invention, the transfer mechanism 4 is arranged on the furnace door 32, so that when ashing is carried out on a plurality of different types of samples, the bracket 33 and the sample crucible in the furnace body 31 are moved to the transfer groove 41 through the sampling block, and then the sample crucible is moved to the outside of the furnace from the transfer groove 41, so that the temperature reduction rate of the sample crucible is slowed down, the problem that the sample crucible is exploded due to the sudden temperature drop is reduced, and meanwhile, different types of samples are borne by different brackets 33, so that when the ashed samples are taken out, the furnace door 32 is not required to be opened, the heat loss in the furnace body 31 is uneven, and the ashing effect of the other types of samples is affected; the ashing completion time of different types of samples can be staggered, and the ashed samples can be detected when the rest samples are ashed, so that the efficiency is improved;
referring to fig. 3, 4 and 5 of the drawings, in this embodiment, a vertical slot 48 is formed at one end of the extraction block 42 near the support 33 in the furnace body 31;
in this embodiment, when the take-out block 42 engages the holder 33, the holder 33 and the sample crucible on the holder 33 are positioned in the vertical groove 48; when the worker finds that the sample is not ashed after taking out the sample crucible, the worker clamps the bracket 33 into the taking-out block 42 again, inserts the taking-out block 42 together with the bracket 33 into the sliding groove 44, pushes forward again, and the bracket 33 is positioned in the vertical groove 48 and cannot contact with the sealing block 43, the taking-out block 42 pushes the sealing block 43 open, the bracket 33 is brought into the furnace, and the bracket 33 is inserted into the sliding groove 34, and at the moment, the worker pulls the steel wire rope 47 and pulls the taking-out block 42 outwards, so that the sample crucible is ashed again in the furnace with the sample;
according to the invention, the support 33 and the sample crucible are placed in the vertical groove 48 on the take-out block 42, so that when the take-out block 42 brings the support 33 and the sample crucible into the furnace body 31 again, the take-out block 42 prevents the support 33 from being contacted with the sealing block 43, and the support 33 and the sample crucible shake, and the sample is shaken out;
referring to fig. 3 and 4 of the drawings, in this embodiment, a plugging plate 49 is rotatably connected to the wall of the sliding groove 44; a drive unit 5 is also arranged below the blocking plate 49;
in this embodiment, the plugging plates 49 are rotatably connected to the side walls on both sides of the sliding groove 44, when the taking-out block 42 is inserted into the sliding groove 44, the taking-out block 42 pushes the plugging plates 49 in the sliding groove 44 to rotate, so that the plugging plates 49 are attached to the inner wall of the sliding groove 44, when the taking-out block 42 is drawn out of the sliding groove 44, the driving unit 5 drives the plugging plates 49 to rotate, and the sliding groove 44 is blocked, so that hot air in the transit groove 41 flows out of the oven door 32 through the sliding groove 44, and further, when a worker pulls out the taking-out block 42, the hot air in the transit groove 41 flows out through the sliding groove 44 and is blown to the hand of the worker, and discomfort or burning of the hand of the worker is caused;
referring to fig. 5 and 6 of the drawings, in the present embodiment, the driving unit 5 includes a weight 51, a cavity 54, a connection string 52, and a through hole 55; the cavity 54 is arranged in the furnace door 32 and is positioned below the transfer groove 41; the weight 51 is located within the cavity 54; the through hole 55 is positioned at the upper end of the cavity 54 and is communicated with the cavity 54; one end of the connecting rope 52 is fixedly connected with the balancing weight 51; the connecting rope 52 below the sealing block 43 is fixedly connected with the sealing block 43; a turntable 53 is rotationally connected below the plugging plate 49, and a connecting rope 52 below the plugging plate 49 is fixedly connected with the outer side surface of the turntable 53; in this embodiment, the connecting cord 52 is made of a wire cord 47;
in this embodiment, the power for driving the closing block 43 and the closing plate 49 to rotate is provided by the gravity of the balancing weight 51, so that when the closing block 43 or the closing plate 49 is pushed by the taking-out block 42, the closing plate 49 and the closing block 43 drive the corresponding turntable 53 to rotate, and when the turntable 53 rotates, the connecting rope 52 is pulled to enable the balancing weight 51 to rise; when the taking-out block 42 is pulled out, the closing block 43 and the plugging plate 49 are not contacted with the taking-out block 42, the balancing weight 51 slides downwards, and the connecting rope 52 is pulled, so that the turntable 53 is reversed to drive the corresponding closing block 43 or the corresponding plugging plate 49 to return to the original position, and the transfer groove 41 or the sliding groove 44 is plugged again;
according to the invention, the closing block 43 and the plugging plate 49 are driven to return to the original positions by the gravity of the balancing weight 51 in the driving unit 5, and meanwhile, the connecting rope 52 is made of the steel wire rope 47, so that the furnace can resist high temperature, and compared with the torsion spring and other components, the furnace can be used for a long time in the high temperature environment of the furnace mouth of the furnace body 31, the situation that the similar torsion spring fails due to the long time in the high temperature environment can not occur, and the use effect of the closing block 43 and the plugging plate 49 is ensured.
Embodiment two:
on the basis of the first embodiment, referring to fig. 3 and 5 of the specification, in this embodiment, the number of the closing blocks 43 is the same as that of the taking-out blocks 42, and the positions of the closing blocks 43 correspond to those of the taking-out blocks 42; the size of the cross section of the closing block 43 is the same as that of the cross section of the taking-out block 42;
in this embodiment, the front sealing block 43 is pushed open each time the taking-out block 42 enters the furnace body 31, so that only a space capable of only moving the taking-out block 42 is exposed between the transfer tank 41 and the furnace body 31, thereby minimizing the heat in the furnace body 31 entering the transfer tank 41 when the sealing block 43 rotates, increasing the temperature of the transfer tank 41, and affecting the cooling rate and effect of the support 33 and the sample crucible when entering the transfer tank 41;
referring to fig. 2 and 3 of the drawings, in this embodiment, the extracting block 42 is formed by a rotary connection between a first block 61 and a second block 62; the first block 61 is disposed away from the furnace body 31 and is capable of rotating downward; the furnace door 32 is provided with a clamping groove 63;
the heating cavity in the furnace body 31 is deeper, so that the length of the taking-out block 42 needs to be longer, and therefore, one end of the taking-out block 42 can be exposed out of the sliding groove 44 on the furnace door 32, thereby affecting the appearance of the ashing furnace 3 and easily generating the collision condition; therefore, in this embodiment, the withdrawing block 42 is configured to be composed of the first block 61 and the second block 62 which are rotationally connected, so that the first block 61 can be rotated downward, so that the first block 61 is embedded into the clamping groove 63 on the oven door 32, and the situation that the withdrawing block 42 extends out of the sliding groove 44 and a large section of the oven door 32 is exposed is avoided, so that the overall appearance of the invention is improved, and the situation that workers collide with the withdrawing block 42 is prevented.
Claims (3)
1. A residual detection experimental device for lead ion standard solution comprises
A pulverizer (1), a baking furnace (2), an ashing furnace (3) and a spectrometer (7); the ashing furnace (3) can be a muffle furnace;
the ashing furnace (3) comprises a furnace body (31) and a furnace door (32); a chute (34) is formed in the furnace body (31); the sample is clamped in the chute (34) through the bracket (33);
the method is characterized in that: a transfer mechanism (4) is arranged on the ashing furnace (3); the transfer mechanism (4) can transfer the bracket (33) and the sample crucible in the ashing furnace (3) into the furnace door (32), so that the temperature reduction rate of the sample crucible is reduced, and the sample crucible is prevented from being fried;
the transfer mechanism (4) comprises a transfer groove (41), a taking-out block (42) and a closing block (43); the transfer groove (41) is formed in the furnace door (32); the furnace door (32) is uniformly provided with sliding grooves (44); the extraction block (42) is slidably connected in the sliding groove (44); one end of the taking-out block (42) close to the inside of the furnace body (31) is arranged in a concave shape and can be clamped with the bracket (33), and one concave end of the taking-out block (42) is rotationally connected with a clamping rod (45); the clamping rod (45) is obliquely arranged; the sealing block (43) is rotatably connected to the end face of the furnace door (32) close to the furnace body (31), and the sealing block (43) can plug the transfer groove (41);
a driving unit (5) is arranged in the furnace door (32) and is used for driving the closing block (43) to rotate; the extraction block (42) is made of a heat-insulating material;
the withdrawing block (42) is provided with a rope hole (46); a steel wire rope (47) is arranged in the rope hole (46); one end of the steel wire rope (47) is fixedly connected with the clamping rod (45), and the other end of the steel wire rope is exposed out of the taking-out block (42);
a vertical groove (48) is formed in one end, close to the bracket (33), of the taking-out block (42) in the furnace body (31); when the withdrawing block (42) is clamped with the bracket (33), the bracket (33) and a sample crucible on the bracket (33) are positioned in the vertical groove (48);
a plugging plate (49) is rotatably connected to the wall of the sliding groove (44); the driving unit (5) is also arranged below the plugging plate (49);
the driving unit (5) comprises a balancing weight (51), a cavity (54), a through hole and a connecting rope (52); the cavity (54) is arranged in the furnace door (32) and is positioned below the transfer groove (41); the balancing weight (51) is positioned in the cavity (54); the through hole is positioned at the upper end of the cavity (54) and is communicated with the cavity (54); one end of the connecting rope (52) is fixedly connected with the balancing weight (51); the connecting rope (52) below the sealing block (43) is fixedly connected with the sealing block (43); a rotary table (53) is rotationally connected below the plugging plate (49), and the connecting rope (52) below the plugging plate (49) is fixedly connected with the outer side surface of the rotary table (53);
the extraction block (42) is formed by rotationally connecting a first block (61) and a second block (62); the first block (61) is arranged far away from the furnace body (31) and can rotate downwards; the furnace door (32) is provided with a clamping groove (63).
2. The device for detecting and testing the residue of the lead ion standard solution according to claim 1, wherein the device comprises: the number of the closing blocks (43) is the same as that of the taking-out blocks (42), and the positions of the closing blocks (43) correspond to those of the taking-out blocks (42); the size of the cross section of the closing block (43) is the same as that of the cross section of the taking-out block (42).
3. A method for detecting the residue of a lead ion standard solution, which is suitable for the experimental device for detecting the residue of the lead ion standard solution according to any one of claims 1 to 2, and is characterized in that: the method comprises the following steps:
s1, placing grain crops into a pulverizer (1) for pulverization, then placing quantitative pulverized grain crop powder into a sample crucible, placing the sample crucible on a baking furnace (2) for baking with small fire to carbonize the sample, placing the sample crucible into a bracket (33), and then placing the sample crucible and the bracket (33) into an ashing furnace (3) for ashing;
s2, after ashing the sample, moving the bracket (33) and the sample crucible to the transfer groove (41) through the taking-out block (42), cooling the bracket (33) and the sample crucible in an environment that the transfer groove (41) is higher than room temperature, and then taking out the taking-out block (42) together with the bracket (33) and the sample crucible from the sliding groove (44);
s3, placing the sample crucible in a room temperature environment for cooling, and adding GR nitric acid into the sample crucible after the sample crucible is cooled to room temperature, wherein the ratio of the GR nitric acid to the sample is 1ml:1g, placing the sample crucible on a heating furnace for evaporating, and adding nitric acid solution and water, wherein the ratio of the nitric acid solution to the water to the sample is 1ML1% nitric acid solution: 3ML water: 1g of sample is placed on a heating furnace again and heated to near boiling by small fire, so that sample solution is obtained; and then the sample solution and an equivalent lead ion standard solution are put into a spectrometer (7) for detection, and the content of lead ions in the sample solution is calculated.
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