CN110208202B - Silver nitrate colorimetric determination method for hydrogen sulfide in workshop air and support frame of porous glass plate absorption tube used for method - Google Patents
Silver nitrate colorimetric determination method for hydrogen sulfide in workshop air and support frame of porous glass plate absorption tube used for method Download PDFInfo
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- CN110208202B CN110208202B CN201910570278.5A CN201910570278A CN110208202B CN 110208202 B CN110208202 B CN 110208202B CN 201910570278 A CN201910570278 A CN 201910570278A CN 110208202 B CN110208202 B CN 110208202B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 112
- 239000005373 porous glass Substances 0.000 title claims abstract description 80
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 title claims abstract description 54
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910001961 silver nitrate Inorganic materials 0.000 title claims abstract description 27
- 230000008093 supporting effect Effects 0.000 claims abstract description 28
- 230000007246 mechanism Effects 0.000 claims abstract description 10
- 239000000523 sample Substances 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 18
- 238000002835 absorbance Methods 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 11
- 238000004737 colorimetric analysis Methods 0.000 claims description 7
- 238000005259 measurement Methods 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000006096 absorbing agent Substances 0.000 claims description 2
- 230000001976 improved effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 5
- 235000019345 sodium thiosulphate Nutrition 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000001230 potassium iodate Substances 0.000 description 2
- 229940093930 potassium iodate Drugs 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- PTLRDCMBXHILCL-UHFFFAOYSA-M sodium arsenite Chemical compound [Na+].[O-][As]=O PTLRDCMBXHILCL-UHFFFAOYSA-M 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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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- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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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
- G01N21/75—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
- G01N21/783—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 for analysing gases
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/02—Mechanical
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Abstract
The invention discloses a colorimetric determination method for silver nitrate of hydrogen sulfide in workshop air and a support frame of a porous glass plate absorption tube used for the method, and the support frame of the porous glass plate absorption tube applied to the colorimetric determination method for the silver nitrate of the hydrogen sulfide in the workshop air comprises a base and two support mechanisms; two limiting grooves for placing U-shaped ends of the porous glass plate absorption tubes are formed in the base; the supporting mechanism comprises a power assembly, a supporting plate, two L-shaped plates and a driving assembly; the vertical ends of the two L-shaped plates are respectively and fixedly connected with the two ends of the supporting plate; the driving assembly comprises a screw rod, a driving unit, a driving plate and a push rod; the screw rod is in threaded connection with the support plate, and the thread directions of two ends of the screw rod are opposite; one end of the push rod, which is far away from the driving plate, abuts against one end of the rubber plug, and the axis of the push rod, the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear. The invention has the advantages of simple operation and improved working efficiency.
Description
Technical Field
The invention relates to the technical field of gas content detection methods, in particular to a silver nitrate colorimetric determination method for hydrogen sulfide in workshop air and a support frame of a porous glass plate absorption tube for the method.
Background
Hydrogen sulfide of the formula H2S, molecular weight is 34.076, it is a flammable acidic gas under standard conditions, colorless, smelly egg smell at low concentration, sulfur smell at very low concentration, and strong toxicity (LC 50=444 ppm)<500 ppm), has a stimulating effect on the respiratory tract and eyes and causes headache, and is dangerous for life at a concentration of 1mg/L or more. The hydrogen sulfide is a flammable and dangerous chemical substance, can form an explosive mixture when being mixed with air, and can cause combustion and explosion when meeting open fire and high heat. Therefore, the content of hydrogen sulfide gas in a workshop needs to be strictly controlled, the existing detection of hydrogen sulfide in the air of the workshop is generally measured by using the national standard GB/T16027-1995 'silver nitrate colorimetric determination method for hydrogen sulfide in the air of the workshop', and the principle is that a tawny silver sulfide colloidal solution is produced by reacting with silver nitrate, and the colorimetric determination is carried out.
In the process of measurement, errors are reduced as much as possible to improve the accuracy of a test result, the collection of a sample is a more critical step for reducing the errors, and the collection method of the sample is generally required to be carried out according to GBZ159-2004 'sampling specification for detecting harmful substances in air of a workplace'; in the silver nitrate colorimetric determination method of hydrogen sulfide, a rubber tube is generally adopted to be connected in series with 2 porous glass plate absorption tubes respectively filled with 10.0mL of absorption liquid at a sampling point, and an air sample is collected for 15min at the flow rate of 0.5L/min; after sampling, the rubber tube is taken down from the porous glass plate absorption tube, and the air inlet and outlet of the porous glass absorption tube are sealed by the rubber plug to reduce air entering the absorption tube. However, such operation is time-consuming, and air is likely to enter the porous glass plate absorption tube during the operation, which increases the test error and affects the working efficiency.
Disclosure of Invention
One of the purposes of the invention is to provide a support frame of a porous glass plate absorption tube, which is applied to a colorimetric determination method of silver nitrate of hydrogen sulfide in workshop air and has the advantages of simple and convenient operation, error reduction and work efficiency improvement.
The technical purpose of the invention is realized by the following technical scheme:
a support frame of a porous glass plate absorption tube applied to a colorimetric determination method of silver nitrate of hydrogen sulfide in workshop air comprises a base and two support mechanisms arranged on the base; the base is provided with two limiting grooves for placing U-shaped ends of the porous glass plate absorption tubes;
the supporting mechanism comprises a power assembly, a supporting plate, two L-shaped plates and a driving assembly;
one end of the power assembly is fixedly arranged on the base, and the other end of the power assembly is fixedly connected with the supporting plate;
the vertical ends of the two L-shaped plates are respectively and fixedly connected with the two ends of the supporting plate, and the L-shaped plates (23) are used for supporting the rubber plug;
the driving assembly comprises a screw rod, a driving unit, a driving plate and a push rod;
the screw rod is rotationally connected to the supporting plate, the thread directions of two ends of the screw rod are opposite, and the axis of the screw rod is perpendicular to the axis of the limiting groove;
one end of the driving unit is fixedly arranged on the supporting plate, and the other end of the driving unit is fixedly connected with the screw rod;
one end of the driving plate is in threaded connection with the screw rod, and the other end of the driving plate is fixedly connected with the push rod;
one end of the push rod, which is far away from the driving plate, abuts against one end of the rubber plug, and the axis of the push rod, the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear.
By adopting the technical scheme, the porous glass plate absorption tube is arranged in the limiting groove on the base for fixing, and the power assembly drives the supporting plate to move up and down, so that the axis of the push rod, the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear; then start drive assembly, make it drive the lead screw and rotate, two threaded connection move towards the direction that is close to the porous glass board absorption tube simultaneously in the drive plate of lead screw this moment, and fixed connection moves towards the horizontal end that is close to the porous glass board absorption tube in the push rod of drive plate, makes the push rod with the rubber buffer propelling movement to the air inlet and the gas outlet of porous glass board absorption tube to can be sealed the both ends of porous glass board absorption tube fast, improved work efficiency.
Furthermore, the power assembly is an air cylinder with one end fixedly connected to the base and the other end fixedly connected to the supporting plate.
Through adopting above-mentioned technical scheme, start the cylinder, make it drive backup pad rebound, easy and simple to handle.
Furthermore, the driving unit is a motor with one end fixedly arranged on the supporting plate and the other end fixedly connected to the screw rod.
By adopting the technical scheme, the motor is started to drive the screw rod to rotate, and the operation is simple and convenient.
Furthermore, the driving assembly further comprises a storage block fixedly arranged on the L-shaped plate, a storage groove is formed in the storage block, a spring is arranged in the storage groove, one end of the spring is fixedly connected to the horizontal end of the L-shaped plate, and the other end of the spring abuts against the rubber plug;
the storage block is provided with a through groove communicated with the storage groove, the rubber plug is arranged in the through groove, the axis of the push rod, the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear, and the push rod can pass through the through groove.
Through adopting above-mentioned technical scheme, locate the rubber buffer in the storing groove of storage piece, can prevent that the push rod from taking place to remove when promoting the rubber buffer, improving the stability of removing.
Further, still be equipped with the bearing block in the storing groove, the bottom fixed connection of bearing block keeps away from the one end of "L" shaped plate in the spring, the top of bearing block is seted up flutedly, and the outer loop face of rubber buffer is laminated on the cambered surface of recess.
Through adopting above-mentioned technical scheme, the recess can play the spacing effect of support to the rubber buffer, reduces the removal of rubber buffer.
Further, the feed chute that communicates in the storing groove is seted up to the lateral wall of storing piece, the feed chute is located the below that leads to the groove, the size of feed chute is greater than the size of rubber buffer.
Through adopting above-mentioned technical scheme, fill in the rubber buffer storing groove from the feed chute, make the storing groove can hold a plurality of rubber grooves simultaneously, can continuously seal porous glass board absorption tube, further improved work efficiency.
The invention also aims to provide a colorimetric determination method for silver nitrate of hydrogen sulfide in workshop air.
The technical purpose of the invention is realized by the following technical scheme:
a colorimetric determination method for silver nitrate of hydrogen sulfide in workshop air comprises the following steps:
(1) collecting a sample: fixing a support frame of the porous glass plate absorption tube on an air extractor; taking two porous glass plate absorption tubes respectively filled with 10mL of absorption liquid, placing the two porous glass plate absorption tubes on a support frame, taking a rubber tube, connecting one end of the rubber tube to an air outlet of one porous glass plate absorption tube, and connecting the other end of the rubber tube to an air inlet of the other porous absorption tube; then, air is pumped out of the porous glass plate absorption tube by an air pump, and a 15min air sample is collected at the flow rate of 0.5L/min;
after sampling, taking the rubber tube out of the porous absorption tube, starting the air cylinder to drive the supporting plate to move upwards, enabling the push rod, the through grooves and the rubber plug to be collinear, then starting the motor to drive the screw rod to rotate, simultaneously moving the two driving plates which are in threaded connection with the screw rod towards the direction close to the porous glass plate absorption tube, moving the push rod fixedly connected with the driving plates towards the direction close to the adjacent through grooves, enabling the push rod to enter the through grooves, pushing the rubber plug in the through grooves to move towards the horizontal end of the porous glass plate absorption tube so as to plug the air inlet and the air outlet of the porous glass plate absorption tube, and then taking the porous glass plate absorption tube out of the base;
(2) and (3) an analysis step:
control test: bringing a porous glass plate absorption tube filled with 10.0mL of absorption liquid to a sampling point, and taking the same sample as a blank control of the sample except that an air extractor is not connected for collecting an air sample;
sample treatment: washing the inner wall of the air inlet pipe of the absorption pipe for 3 times by using the sampled absorption liquid; 5.0mL of absorption solution is taken from the front tube and the rear tube respectively and put into a colorimetric tube with a plug, and the tubes are shaken up for determination; if the concentration of the substance to be measured in the sample liquid exceeds the measuring range, measuring after diluting by using absorption liquid, and multiplying by the dilution times during calculation;
drawing a standard curve: taking 10 colorimetric tubes with plugs, respectively adding 0.0, 0.10, 0.20, 0.30, 0.40, 0.50, 0.60, 0.70, 0.80 and 1.00mL of hydrogen sulfide standard solution, adding the absorption solution to 5.0mL respectively, and preparing into 0.0, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0, 14.0, 16.0 and 20.0 mu g of hydrogen sulfide standard series; adding 0.2mL of starch solution into each standard tube, and shaking up; adding 1.0mL of silver nitrate solution; shaking, standing for 5min, and performing color comparison;
(3) and (3) calculating: calculating the concentration of hydrogen sulfide in the air according to the following formula;
X=
in the formula: concentration of hydrogen sulfide in X-air, mg/m3；
m1，m2-measuring the hydrogen sulphide content, μ g, in the front and rear tube samples;
V0-a standard sample volume, L.
Further, the color comparison in the step (2) is carried out by using an ultraviolet visible spectrophotometer.
By adopting the technical scheme, the ultraviolet-visible spectrophotometer is an analyzer for analyzing by utilizing the radiation absorption of substance molecules to an ultraviolet-visible spectrum region based on the principle of an ultraviolet-visible spectrophotometry, each substance has a specific and fixed absorption spectrum curve, the content of the substance can be determined according to the absorbance at certain special wavelengths on the absorption spectrum, and compared with visual colorimetry, the ultraviolet-visible spectrophotometer can improve the accuracy of colorimetry and is favorable for reducing errors.
Further, the colorimetric method specifically comprises the following steps: measuring absorbance at 400nm wavelength by using an ultraviolet-visible spectrophotometer, repeatedly measuring each concentration for 3 times, and drawing a standard curve by using the absorbance average value to the corresponding hydrogen sulfide content (mu g); measuring the sample solution and the blank control solution by using the operation conditions of the measurement standard series; after subtracting the absorbance value of the blank control from the absorbance value of the sample, the hydrogen sulfide content (μ g) was obtained from the standard curve.
In summary, compared with the prior art, the invention has the following beneficial effects:
1. the support frame can automatically seal the porous glass plate absorption tube after sampling, the operation is simple and convenient, the working efficiency is improved, and the porous glass plate absorption tube is also beneficial to storage and transportation after being sealed;
2. the ultraviolet-visible spectrophotometer is an analytical instrument for analyzing by utilizing radiation absorption of substance molecules to an ultraviolet-visible spectrum region based on the principle of an ultraviolet-visible spectrophotometry, each substance has a specific and fixed absorption spectrum curve, the content of the substance can be determined according to the absorbance at certain special wavelengths on the absorption spectrum, and compared with visual colorimetry, the ultraviolet-visible spectrophotometer can improve the accuracy of the colorimetry and is beneficial to reducing errors.
Drawings
FIG. 1 is a schematic view showing the overall structure of a support frame of the absorber tube for a multi-well glass panel in this example 1;
FIG. 2 is a partial structural view of a receiving block highlighted in embodiment 1;
FIG. 3 is a schematic sectional view of the storage tank highlighted in example 1.
In the figure, 1, a base; 11. a limiting groove; 2. a support mechanism; 21. a power assembly; 211. a cylinder; 22. a support plate; 23. an "L" shaped plate; 24. a drive assembly; 241. a drive unit; 2411. a motor; 242. a drive plate; 243. a push rod; 244. storing the material blocks; 2441. a storage tank; 2442. a spring; 2443. a bearing block; 2444. a through groove; 2445. a groove; 2446. a feed chute; 245. and a screw rod.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1: referring to fig. 1, the support frame for a porous glass plate absorption tube disclosed by the invention comprises a rectangular base 1 and two support mechanisms 2 arranged on the base, wherein two limiting grooves 11 for placing U-shaped ends of the porous glass plate absorption tube are formed in the base 1 along the vertical direction, the two limiting grooves 11 are in the same plane, and the support mechanisms 2 are arranged on one sides of the limiting grooves 11.
Referring to fig. 1, the supporting mechanism 2 includes a power assembly 21, a supporting plate 22, two "L" shaped plates 23 and a driving assembly 24, where the power assembly 21 includes two (but not limited to two) cylinders 211 fixed on the base 1, and one end of the cylinder 211 away from the base 1 is fixedly connected to the supporting plate 22; the vertical ends of the two "L" shaped plates 23 are fixedly connected to the two ends of the support plate 22, respectively.
Referring to fig. 2 and 3, the driving assembly 24 includes a screw 245, a driving unit 241, a driving plate 242, a push rod 243 and a storage block 244, the screw 245 is rotatably connected to the supporting plate 22, and the directions of the threads at the two ends of the screw are opposite, and the axis of the screw 245 is perpendicular to the axis of the limiting groove 11; the screw 245 is positioned above the "L" shaped plate 23; the driving unit 241 comprises a motor 2411 fixedly arranged on the supporting plate 22, and an output shaft of the motor 2411 is fixedly connected to one end of the screw 245; the driving plate 242 is in threaded connection with the screw rod 245, and one end of the driving plate 242, which is far away from the screw rod 245, is fixedly connected with the push rod 243; the bottom end of the storage block 244 is fixedly connected to the L-shaped plate 23, a storage groove 2441 is formed in the storage block 244, two (but not limited to two) springs 2442 and a bearing block 2443 are arranged in the storage groove 2441, a through groove 2444 communicated with the storage groove 2441 is formed in the storage block 244, the axis of the through groove 2444, the axis of the push rod 243, the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear, and the push rod 243 can pass through the through groove 2444; one end of the spring 2442 is fixedly connected with the horizontal end of the L-shaped plate 23, the other end of the spring 2442 is fixedly connected with the bearing block 2443, one end of the bearing block 2443, which is far away from the spring 2442, is provided with a groove 2445, and the outer annular surface of the rubber plug is attached to the cambered surface of the groove 2445; the spring 2442, the bearing block 2443 and the rubber plug are all arranged in the storage groove 2441; the side wall of the storage block 244 is provided with a feed chute 2446 communicated with the storage chute 2441, the feed chute 2446 is positioned below the through chute 2444, and the size of the feed chute 2446 is slightly larger than that of the rubber stopper.
The implementation principle of the embodiment is as follows: before the test, two (but not limited to two) rubber plugs are taken and plugged from the feeding groove 2446 of the storage block 244, the outer ring surfaces of the rubber plugs are attached to the cambered surface of the groove 2445, the spring 2442 is compressed at the moment, and the axes of the rubber plugs are collinear with the axes of the through grooves 2444 under the action of the elastic force of the spring 2442; the operation is repeated, and another rubber plug is plugged, so that a plurality of rubber plugs are accommodated in the storage groove 2441 at the same time.
The U-shaped ends of the two porous glass plate absorption tubes are respectively arranged in the limiting grooves 11 on the base 1 so as to fix the two porous glass plate absorption tubes, and the cylinder 211 is started to drive the supporting plate 22 to move downwards so that the push rod is positioned at the lower side of the horizontal end of the porous glass plate absorption tube; then one end of the rubber hose is communicated with an air outlet of one porous glass plate absorption tube, and the other end of the rubber hose is communicated with an inlet and an outlet of the other porous glass plate absorption tube, so that the two porous glass plate absorption tubes are connected in series; then an air extractor is connected with an air inlet of the porous glass plate absorption tube, so that air enters the porous glass plate absorption tube to collect a sample.
After sampling, the rubber tube is taken out of the porous absorption tube, the cylinder 211 is started to drive the support plate 22 to move upwards, the push rod 243, the through groove 2444 and the rubber plug are collinear, then the motor 2411 is started to drive the screw rod 245 to rotate, at the moment, the two drive plates 242 which are in threaded connection with the screw rod 245 simultaneously move towards the direction close to the porous glass plate absorption tube, the push rod 243 fixedly connected to the drive plates 242 moves towards the direction close to the adjacent through groove 2444, the push rod 243 enters the through groove 2444, the rubber plug in the through groove 2444 is pushed to move towards the horizontal end of the porous glass plate absorption tube, so that the air inlet and the air outlet of the porous glass plate absorption tube are blocked, and then the porous glass plate absorption tube is taken out of the base.
Example 2: silver nitrate colorimetric determination method for hydrogen sulfide in workshop air
(1) Reagent preparation
Absorbing liquid: 2g of sodium arsenite (NaAsO) are dissolved2) Diluting with water to 1000mL in 100mL ammonium carbonate solution (50 g/L);
starch solution, 10 g/L: dissolving 1g of soluble starch in 10mL of cold water, uniformly stirring, slowly pouring into 90mL of boiling water, stirring while adding, and boiling for 1 min; cooling for later use;
③ silver nitrate solution 10 g/L: dissolving 1g of silver nitrate in 90mL of water, and adding 10mL of sulfuric acid (. rho.201.84 g/mL), if precipitate is generated in the standing process, filtering is needed;
sodium thiosulfate solution: 25g of sodium thiosulfate (Na) are weighed2S2O3•5H2O), dissolving in boiled and cooled water, transferring into a 1000mL volumetric flask, adding 0.4g of sodium hydroxide, and adding water to the scale;
calibration: accurately weighing 0.1500g potassium iodate (dried at 105 deg.C for 30 min) in a 250mL iodine bottle, adding 100mL water, and heating to dissolve; after cooling, adding 3g of potassium iodide and 10mL of glacial acetic acid to generate iodine, wherein the solution is brown; quickly titrating with sodium thiosulfate solution until the color becomes yellowish, adding 1mL of starch solution, and continuously titrating until the blue color fades. The sodium thiosulfate concentration was calculated by formula (1):
C=
………………（1）
in the formula: concentration of C-sodium thiosulfate solution, mol/L;
mass of m-potassium iodate, g;
amount of v-sodium thiosulfate used, mL.
The standard solution: 6.0mL of a sodium thiosulfate solution (0.1mol/L) was taken in a 100mL volumetric flask and diluted to the mark with boiling and cooling water. This solution corresponds to a standard stock solution of 0.20 mg/mL hydrogen sulfide; before use, diluting the solution into a hydrogen sulfide standard solution of 20.0 mu g/mL by using absorption liquid;
(2) collecting a sample: fixing a support frame of the porous glass plate absorption tube on an air extractor; taking two porous glass plate absorption tubes respectively filled with 10mL of absorption liquid, placing the two porous glass plate absorption tubes on a support frame, taking a rubber tube, connecting one end of the rubber tube to an air outlet of one porous glass plate absorption tube, and connecting the other end of the rubber tube to an air inlet of the other porous absorption tube; then, air is pumped out of the porous glass plate absorption tube by an air pump, and a 15min air sample is collected at the flow rate of 0.5L/min;
after sampling, taking the rubber tube out of the porous absorption tube, starting the air cylinder 211 to drive the support plate 22 to move upwards, enabling the push rod 243, the through groove 2444 and the rubber plug to be collinear, then starting the motor 2411 to drive the screw rod 245 to rotate, simultaneously moving the two drive plates 242 which are in threaded connection with the screw rod 245 towards the direction close to the porous glass plate absorption tube, moving the push rod 243 fixedly connected to the drive plates 242 towards the direction close to the adjacent through groove 2444, enabling the push rod 243 to enter the through groove 2444, pushing the rubber plug in the through groove 2444 to move towards the horizontal end of the porous glass plate absorption tube so as to block the air inlet and the air outlet of the porous glass plate absorption tube, and then taking the porous glass plate absorption tube out of the base 1;
(3) and (3) an analysis step:
control test: bringing a porous glass plate absorption tube filled with 10.0mL of absorption liquid to a sampling point, and taking the same sample as a blank control of the sample except that an air extractor is not connected for collecting an air sample;
sample treatment: washing the inner wall of the air inlet pipe of the absorption pipe for 3 times by using the sampled absorption liquid; 5.0mL of absorption solution is taken from the front tube and the rear tube respectively and put into a colorimetric tube with a plug, and the tubes are shaken up for determination; if the concentration of the substance to be measured in the sample liquid exceeds the measuring range, measuring after diluting by using absorption liquid, and multiplying by the dilution times during calculation;
drawing a standard curve: taking 10 colorimetric tubes with plugs, respectively adding 0.0, 0.10, 0.20, 0.30, 0.40, 0.50, 0.60, 0.70, 0.80 and 1.00mL of hydrogen sulfide standard solution, adding the absorption solution to 5.0mL respectively, and preparing into 0.0, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0, 14.0, 16.0 and 20.0 mu g of hydrogen sulfide standard series; adding 0.2mL of starch solution into each standard tube, and shaking up; adding 1.0mL of silver nitrate solution; shaking, standing for 5min, performing colorimetry with ultraviolet-visible spectrophotometer, measuring absorbance at 400nm wavelength, repeating the measurement for 3 times for each concentration, and drawing a standard curve of the absorbance average value to corresponding hydrogen sulfide content (μ g); measuring the sample solution and the blank control solution by using the operation conditions of the measurement standard series; subtracting the blank control absorbance value from the measured sample absorbance value, and obtaining the content (mu g) of the hydrogen sulfide from the standard curve;
(4) and (3) calculating: the sample volume was converted to the standard volume according to equation (2):
V0=V×
×
………………（2）
in the formula: v0-sample volume under standard conditions, L;
v-sample volume, L;
t-temperature, DEG C;
p-atmospheric pressure, kPa;
calculating the concentration of hydrogen sulfide in the air according to the formula (3);
X=
………………（3）
in the formula: concentration of hydrogen sulfide in X-air, mg/m3；
m1，m2-measuring the hydrogen sulphide content, μ g, in the front and rear tube samples;
V0-a standard sampling volume, L;
(5) description of the invention
The detection limit of the method is 0.4 mug/mL; the lowest detected concentration is 0.53mg/m3(to take a 7.5L air sample); the measurement range is 0.4 to 4 μ g/mL. The mean relative standard deviation was 3.4%;
② sulfides interfere with the measurement.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (9)
1. A support frame of a porous glass plate absorption tube for a colorimetric determination method of silver nitrate of hydrogen sulfide in workshop air is characterized in that: comprises a base (1) and two supporting mechanisms (2) arranged on the base (1); the base (1) is provided with two limiting grooves (11) for placing U-shaped ends of the porous glass plate absorption tubes;
the supporting mechanism (2) comprises a power assembly (21), a supporting plate (22), two L-shaped plates (23) and a driving assembly (24);
one end of the power component (21) is fixedly arranged on the base (1), and the other end of the power component is fixedly connected with the supporting plate (22);
the vertical ends of the two L-shaped plates (23) are respectively and fixedly connected with the two ends of the supporting plate (22), and the L-shaped plates (23) are used for supporting the rubber plug;
the driving assembly (24) comprises a screw rod (245), a driving unit (241), a driving plate (242) and a push rod (243);
the screw rod (245) is rotatably connected to the support plate (22), the directions of the threads at the two ends of the screw rod are opposite, and the axis of the screw rod (245) is vertical to the axis of the limiting groove (11);
one end of the driving unit (241) is fixedly arranged on the supporting plate (22), and the other end of the driving unit is fixedly connected with the screw rod (245);
one end of the driving plate (242) is connected with the screw rod (245) in a threaded manner, and the other end of the driving plate is fixedly connected with the push rod (243);
one end of the push rod (243) far away from the driving plate (242) is abutted against one end of the rubber plug, and the axis of the push rod (243), the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear.
2. The support frame of the porous glass plate absorption tube for the colorimetric determination method of silver nitrate in hydrogen sulfide in workshop air as claimed in claim 1, characterized in that: the power assembly (21) is a cylinder (211) with one end fixedly connected to the base (1) and the other end fixedly connected to the support plate (22).
3. The support frame of the porous glass plate absorption tube for the colorimetric determination method of silver nitrate in hydrogen sulfide in workshop air as claimed in claim 1, characterized in that: the driving unit (241) is a motor (2411) with one end fixedly arranged on the supporting plate (22) and the other end fixedly connected to the screw rod (245).
4. The support frame of the porous glass plate absorption tube for the colorimetric determination method of silver nitrate in hydrogen sulfide in workshop air as claimed in claim 2, characterized in that: the driving assembly (24) further comprises a storage block (244) fixedly arranged on the L-shaped plate (23), a storage groove (2441) is formed in the storage block (244), a spring (2442) is arranged in the storage groove (2441), one end of the spring (2442) is fixedly connected to the horizontal end of the L-shaped plate (23), and the other end of the spring abuts against the rubber plug;
a through groove (2444) communicated with the storage groove (2441) is formed in the storage block (244), the rubber plug is arranged in the through groove (2444), the axis of the push rod (243), the axis of the rubber plug and the axis of the horizontal end of the porous glass plate absorption tube are collinear, and the push rod (243) can penetrate through the through groove (2444).
5. The support frame of the porous glass plate absorption tube for the colorimetric determination method of silver nitrate in hydrogen sulfide in workshop air as claimed in claim 4, characterized in that: the storage groove (2441) is also internally provided with a bearing block (2443), the bottom end of the bearing block (2443) is fixedly connected to one end, far away from the L-shaped plate (23), of the spring (2442), the top end of the bearing block (2443) is provided with a groove (2445), and the outer annular surface of the rubber plug is attached to the arc surface of the groove (2445).
6. The support frame of the porous glass plate absorption tube for the colorimetric determination method of silver nitrate in hydrogen sulfide in workshop air as claimed in claim 4, characterized in that: the lateral wall of storage piece (244) is seted up feed chute (2446) that communicates in storage groove (2441), feed chute (2446) are located the below of logical groove (2444), the size of feed chute (2446) is greater than the size of rubber buffer.
7. A colorimetric determination method of silver nitrate of hydrogen sulfide in plant air using a support frame of a porous glass plate absorber tube as claimed in any one of claims 4 to 6, characterized in that: the method comprises the following steps:
(1) collecting a sample: fixing a support frame of the porous glass plate absorption tube on an air extractor; taking two porous glass plate absorption tubes respectively filled with 10mL of absorption liquid, placing the two porous glass plate absorption tubes on a support frame, taking a rubber tube, connecting one end of the rubber tube to an air outlet of one porous glass plate absorption tube, and connecting the other end of the rubber tube to an air inlet of the other porous absorption tube; then, air is pumped out of the porous glass plate absorption tube by an air pump, and a 15min air sample is collected at the flow rate of 0.5L/min;
after sampling, taking the rubber tube out of the porous absorption tube, starting the air cylinder (211) to drive the support plate (22) to move upwards, enabling the push rod (243), the through grooves (2444) and the rubber plugs to be collinear, then starting the motor (2411) to drive the screw rod (245) to rotate, enabling the two drive plates (242) which are in threaded connection with the screw rod (245) to simultaneously move towards the direction close to the porous glass plate absorption tube, enabling the push rod (243) fixedly connected to the drive plates (242) to move towards the direction close to the adjacent through grooves (2444), enabling the push rod (243) to enter the through grooves (2444), pushing the rubber plugs in the through grooves (2444) to move towards the horizontal end of the porous glass plate absorption tube so as to block the air inlets and the air outlets of the porous glass plate absorption tube, and then taking the porous glass plate absorption tube out of the base (1);
(2) and (3) an analysis step:
control test: bringing a porous glass plate absorption tube filled with 10.0mL of absorption liquid to a sampling point, and taking the same sample as a blank control of the sample except that an air extractor is not connected for collecting an air sample;
sample treatment: washing the inner wall of the air inlet pipe of the absorption pipe for 3 times by using the sampled absorption liquid; 5.0mL of absorption solution is taken from the front tube and the rear tube respectively and put into a colorimetric tube with a plug, and the tubes are shaken up for determination; if the concentration of the substance to be measured in the sample liquid exceeds the measuring range, measuring after diluting by using absorption liquid, and multiplying by the dilution times during calculation;
drawing a standard curve: taking 10 colorimetric tubes with plugs, respectively adding 0.0, 0.10, 0.20, 0.30, 0.40, 0.50, 0.60, 0.70, 0.80 and 1.00mL of hydrogen sulfide standard solution, adding the absorption solution to 5.0mL respectively, and preparing into 0.0, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0, 14.0, 16.0 and 20.0 mu g of hydrogen sulfide standard series; adding 0.2mL of starch solution into each standard tube, and shaking up; adding 1.0mL of silver nitrate solution; shaking, standing for 5min, and performing color comparison;
(3) and (3) calculating: calculating the concentration of hydrogen sulfide in the air according to the following formula;
X=
in the formula: concentration of hydrogen sulfide in X-air, mg/m3；
m1，m2-measuring the hydrogen sulphide content, μ g, in the front and rear tube samples;
V0-a standard sample volume, L.
8. The method for the colorimetric determination of silver nitrate in hydrogen sulfide in plant air as claimed in claim 7, wherein: and (3) carrying out color comparison by adopting an ultraviolet visible spectrophotometer in the step (2).
9. The method for the colorimetric determination of silver nitrate in hydrogen sulfide in plant air as claimed in claim 7, wherein: the colorimetric method comprises the following steps: measuring absorbance at 400nm wavelength by using an ultraviolet-visible spectrophotometer, repeatedly measuring each concentration for 3 times, and drawing a standard curve by using the absorbance average value to the corresponding hydrogen sulfide content (mu g); measuring the sample solution and the blank control solution by using the operation conditions of the measurement standard series; after subtracting the absorbance value of the blank control from the absorbance value of the sample, the hydrogen sulfide content (μ g) was obtained from the standard curve.
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