CN104990884A - Method for detecting manganese and manganese inorganic compounds in air of operation environment - Google Patents
Method for detecting manganese and manganese inorganic compounds in air of operation environment Download PDFInfo
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Abstract
The invention provides a method for detecting manganese and manganese inorganic compounds in air of an operation environment. First glass fiber filter paper is made to be charged with negative electricity, and second glass fiber filter paper is made to be charged with positive electricity; an insulating clearance is preserved between the first glass fiber filter paper and the second glass fiber filter paper for sampling; it is guaranteed that the windward side of the first glass fiber filter paper and the windward side of the second glass fiber filter paper are upward, a first beaker is placed in slowly and stably, and phosphoric acid is added and dissolved completely; clear water is added to the first beaker for attenuation and heated, and then the solution is filtered; a part of solution to be measured arranged in a second colorimetric tube; a blank fourth colorimetric tube and multiple sets of standard tubes containing manganese dioxide standard solutions of different contents are made; potassium periodate is added to the second colorimetric tube, the fourth colorimetric tube and all the standard tubes, and all the tubes are heated in a boiling water bath until all solutions reach spectrophotometry colorimetric conditions; colorimetric assay is carried out. Therefore, the method can accurately an effectively detect manganese and manganese inorganic compounds in the air of the operation environment.
Description
Technical field
The present invention relates to the detection method field of manganese and mineral compound content thereof in air, be specifically related to a kind of method detecting manganese and mineral compound content thereof in operating environment air.
Background technology
Manganese is one of trace element of needed by human, and manganese deficiency can cause skeleton teratogenesis, artery sclerosis, but excess intake also can cause manganese poisoning, makes central nervous system undermined.Therefore in the operating environment air especially closed of testing environment, the content of manganese and mineral compound thereof is significant.
The detection method of manganese and mineral compound thereof has been known, as Chinese invention patent CN 201410473900.8 discloses the detection method of trace manganese in a kind of environmental sample, comprise the following steps: take environmental sample 0.200g in quartz beaker, add the pure nitric acid low temperature of 10mL top grade to clear up, treat organic Colors from brown become faint yellow, add 1mL perchloric acid to continue to clear up, emit to the greatest extent to white cigarette, solution is closely dry, cool the nitric acid dissolve of rear 25mL1%, then 1mL5% potassium metaperiodate is added, 2mL red fuming nitric acid (RFNA), heating is boiled, to there is after blush micro-3min that boils again, above-mentioned solution pH value is adjusted to 3, pour in the conical flask that the shitosan CCTS of 30mg after epichlorokydrin is cross-linked is housed, in constant-temperature table vibration 30min, filter, by the shitosan CCTS after epichlorokydrin is cross-linked after absorption, with 10 10% oxammonium hydrochloride wash-outs, be settled to 5m1, with the content of Flame Atomic Absorption Spectrometry Determination manganese.The preparation method of the described shitosan CCTS after epichlorokydrin is cross-linked takes 6.0g soluble chitosan to be dissolved in the acetum of 320mL1%, while vigorous stirring, slowly add 6mL epichlorokydrin, drip the NaOH of 50mL 5% gradually, continue reaction 18h, until generate a white solid, after suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing, drying, mill, is for subsequent use after the screening of 0.075mm sub-sieve with aperture.The condition of work of described flame atomic absorption spectrometry is wavelength 279.5nm, lamp current 4mA, spectral band-width 0.05mm, acetylene flow 1.6L/min, air mass flow 7-5L/min.The method can not detect the concrete content of manganese and mineral compound thereof in operating environment air accurately and efficiently in actual application, qualitative especially quantitatively on cannot reach detection demand, accuracy and practicality have much room for improvement.
Given this, inventor furthers investigate the problems referred to above, then has this case to produce.
Summary of the invention
The object of the present invention is to provide a kind of can smooth and easy quick realization sampling and the whole flow process that detects, reach the method for manganese and mineral compound content thereof in the detection operating environment air of manganese and mineral compound content detection thereof in accurate operating environment air efficiently, flow process is succinct, practical.
In order to achieve the above object, the present invention adopts such technical scheme:
Detect a method for manganese and mineral compound content thereof in operating environment air, comprise the steps:
(1) get glass fiber filter paper two panels, adopt friction or electron stream method of radiating to make the first glass fiber filter paper electronegative, adopt friction or positive ion stream method of radiating to make the second glass fiber filter paper positively charged;
(2) by the first glass fiber filter paper and the suction opeing of the parallel block of the second glass fiber filter paper at metering aspirator, and keep, between the first glass fiber filter paper and the second glass fiber filter paper, there is clearance for insulation;
(3) record operating environment air themperature and air pressure, open metering aspirator and sample with wind speed a1 extracting air volume a2;
(4) after sampling terminates, first glass fiber filter paper and the second glass fiber filter paper are taken off, and ensure that windward side is upward, slowly steadily put into first beaker of volume b1, ensure that the particle that the first glass fiber filter paper and the second glass fiber filter paper are adsorbed can not drop;
(5) in the first beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the first beaker is heated, and carry out stirring or shearing, the first glass fiber filter paper and the second glass fiber filter paper are dissolved completely;
(6) the first beaker is cooled to temperature b6; If now pitchy appears in solution, add the ammonium nitrate of concentration b7, volume b8, then with programming rate b9, the first beaker is heated, until yellow gas overflows completely;
(7) in the first beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted;
(8) with programming rate c2, the first beaker is heated, make the first beaker reach temperature c3 and retention time c4;
(9) with filter paper, the solution in the first beaker is filtered while keeping the first beaker temperature c3, contaminant filter is fallen, and make solution directly fall into first color comparison tube of volume d1, and with the clear water of volume d2, the first beaker, filter paper and impurity are rinsed, make washing fluid also flow in the first color comparison tube, measure overall solution volume d3;
(10) in the first color comparison tube, the solution to be measured of volume d4 is got in the second color comparison tube;
(11) the 3rd glass fiber filter paper of blank and the 4th glass fiber filter paper are put into second beaker of volume b1;
(12) in the second beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the second beaker is heated, and carry out stirring or shearing, the 3rd glass fiber filter paper and the 4th glass fiber filter paper are dissolved completely;
(13) the second beaker is cooled to temperature b6;
(14) in the second beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted;
(15) with programming rate c2, the second beaker is heated, make the second beaker reach temperature c3 and retention time c4;
(16) with filter paper, the solution in the second beaker is filtered while keeping the second beaker temperature c3, contaminant filter is fallen, and make solution directly fall into the 3rd color comparison tube of volume d1, and with the clear water of volume d2, the second beaker, filter paper and impurity are rinsed, make washing fluid also flow in the 3rd color comparison tube, measure overall solution volume d3;
(17) in the solution getting volume d4 in the 3rd color comparison tube and the 4th color comparison tube;
(18) standard solution of the many groups of configuration containing variable concentrations manganese dioxide is in multiple standard pipe;
(19) in above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe, add the potassium metaperiodate of weight e1 respectively;
(20) by above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe heat time e2 in boiling water bath, and stir, until each solution reaches spectrophotometric colorimetric condition, take out and be cooled to temperature b6;
(21) under the illumination of wavelength 530nm, colorimetric assay is carried out;
(22) utilize the colorimetric assay value drawing standard curve of the standard solution in each standard pipe, the colorimetric assay value then contrasted in the second color comparison tube and the 4th color comparison tube extrapolates the levels of manganese in operating environment air and mineral compound thereof.
In above-mentioned steps (2), above-mentioned first glass fiber filter paper is in the upstream of air-flow direction, and above-mentioned second glass fiber filter paper is in the downstream of air-flow direction.
Repeat corresponding steps, make many groups the second color comparison tube, extrapolate the levels of manganese in many group jobs surrounding air and mineral compound thereof, then average.
Above-mentioned wind speed a1 is 8-12L/min; Above-mentioned volume a2 is 800-1200L; Above-mentioned volume b1 is 60-80ml; Above-mentioned concentration b2 is volumetric concentration 80-90%; Above-mentioned volume b3 is 8-12ml; Said temperature b4 is 245-250 DEG C; Above-mentioned time b5 is 3-10 minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is 10-30mg/ml; Above-mentioned volume b8 is 0.05-0.5ml; Above-mentioned programming rate b9 is 2-5 DEG C/min; Above-mentioned volume c1 is 20-30ml; Above-mentioned programming rate c2 is 10-20 DEG C/min; Said temperature c3 is 90-95 DEG C; Above-mentioned time c4 is 2-3 minute; Above-mentioned volume d1 is 40-60ml; Above-mentioned volume d2 is 4-10ml; Above-mentioned volume d3 is 40-60ml; Above-mentioned volume d4 is 20-25ml; Above-mentioned weight e1 is 0.25-0.3g; Above-mentioned time e2 is 25-30 minute.
Above-mentioned wind speed a1 is 9.5-10.5L/min; Above-mentioned volume a2 is 950-1050L; Above-mentioned volume b1 is 65-75ml; Above-mentioned concentration b2 is volumetric concentration 84-86%; Above-mentioned volume b3 is 9.5-10.5ml; Said temperature b4 is 247-248 DEG C; Above-mentioned time b5 is 5-7 minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is 15-25mg/ml; Above-mentioned volume b8 is 0.1-0.3ml; Above-mentioned programming rate b9 is 3-4 DEG C/min; Above-mentioned volume c1 is 24-26ml; Above-mentioned programming rate c2 is 14-16 DEG C/min; Said temperature c3 is 92-93 DEG C; Above-mentioned time c4 is 2.3-2.7 minute; Above-mentioned volume d1 is 45-55ml; Above-mentioned volume d2 is 6-8ml; Above-mentioned volume d3 is 45-55ml; Above-mentioned volume d4 is 22-23ml; Above-mentioned weight e1 is 0.27-0.28g; Above-mentioned time e2 is 27-28 minute.
The aperture size of above-mentioned glass fiber filter paper is 0.6-0.9um.
In above-mentioned steps (20), above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe are taken out after boiling water bath, before developing the color, leave standstill 1.5-2.5 hour.
In above-mentioned steps (20), if the solution to be measured in above-mentioned second color comparison tube is purple, dropwise instill with hydrogen peroxide, until color fade, and measure the absorbance of chromium ion, finally deduct the absorbance of chromium ion by total absorbance value, to get rid of the impact of chromium ion on testing result.
Adopt after technique scheme, compared with prior art, the present invention can smooth and easy quick realization sampling and the whole flow process that detects, and reach accurately manganese and mineral compound content detection thereof in operating environment air efficiently, flow process is succinct, practical.
Embodiment
In order to explain technical scheme of the present invention further, be described in detail below by specific embodiment.
A kind of method detecting manganese and mineral compound content thereof in operating environment air of the present invention, comprises the steps:
(1) get glass fiber filter paper two panels, adopt friction or electron stream method of radiating to make the first glass fiber filter paper electronegative, adopt friction or positive ion stream method of radiating to make the second glass fiber filter paper positively charged.Because the molecules such as the dust in air are substantially all polar particulate, can utilize the glass fiber filter paper of static electrification while utilizing micropore to filter particle, also Electrostatic Absorption is carried out to particle, drop after avoiding particle to be adsorbed, or partial particulate is fled from through after filter paper, the accuracy of detection of final manganese and mineral compound thereof can be affected; And both sides glass fiber filter paper can carry out reinforced filtration, and the first glass fiber filter paper and the second glass fiber filter paper electronegative and positive electricity respectively, in time the more weak or obvious particle of the not obvious and aobvious negative electricity of aobvious positive electricity of a small amount of polarity is escaped from the first glass fiber filter paper, also can be adsorbed by the second glass fiber filter paper of positively charged, particle in the air of all samplings of further guarantee is sampled completely, and then guarantees the accuracy of detection of final manganese and mineral compound thereof.
(2) by the first glass fiber filter paper and the suction opeing of the parallel block of the second glass fiber filter paper at metering aspirator, and keep, between the first glass fiber filter paper and the second glass fiber filter paper, there is clearance for insulation.Namely the first glass fiber filter paper and the second glass fiber filter paper can be isolated like this, avoid the two electricity cancel out each other and lose adsorption effect.
(3) record operating environment air themperature and air pressure, open metering aspirator and sample with wind speed a1 extracting air volume a2.
(4) after sampling terminates, first glass fiber filter paper and the second glass fiber filter paper are taken off, and ensure that windward side upward, slowly steadily put into first beaker of volume b1, such method of operating can ensure that the particle that the first glass fiber filter paper and the second glass fiber filter paper are adsorbed can not loosen because of gravity or air flowing, guarantees that the particle that the first glass fiber filter paper and the second glass fiber filter paper are adsorbed can not drop.
(5) in the first beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the first beaker is heated, and carry out stirring or shearing, the first glass fiber filter paper and the second glass fiber filter paper are dissolved completely.
(6) the first beaker is cooled to temperature b6; If now pitchy appears in solution, add the ammonium nitrate of concentration b7, volume b8, then with programming rate b9, the first beaker is heated, until yellow gas overflows completely.Other kations affecting testing result can be rejected by this step.
(7) in the first beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted.
(8) with programming rate c2, the first beaker is heated, make the first beaker reach temperature c3 and retention time c4.This step matches with step (7) and manganese ion can be made to dissolve completely.
(9) with filter paper, the solution in the first beaker is filtered while keeping the first beaker temperature c3, contaminant filter is fallen, and make solution directly fall into first color comparison tube of volume d1, and with the clear water of volume d2, the first beaker, filter paper and impurity are rinsed, make washing fluid also flow in the first color comparison tube, measure overall solution volume d3.This step can reject the impurity such as precipitation, and ensures that all manganese ions all enter in the first color comparison tube, guarantees subsequent detection precision.
(10) in the first color comparison tube, the solution to be measured of volume d4 is got in the second color comparison tube.
(11) the 3rd glass fiber filter paper of blank and the 4th glass fiber filter paper are put into second beaker of volume b1.
(12) in the second beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the second beaker is heated, and carry out stirring or shearing, the 3rd glass fiber filter paper and the 4th glass fiber filter paper are dissolved completely.
(13) the second beaker is cooled to temperature b6.
(14) in the second beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted.
(15) with programming rate c2, the second beaker is heated, make the second beaker reach temperature c3 and retention time c4.
(16) with filter paper, the solution in the second beaker is filtered while keeping the second beaker temperature c3, contaminant filter is fallen, and make solution directly fall into the 3rd color comparison tube of volume d1, and with the clear water of volume d2, the second beaker, filter paper and impurity are rinsed, make washing fluid also flow in the 3rd color comparison tube, measure overall solution volume d3.
(17) in the solution getting volume d4 in the 3rd color comparison tube and the 4th color comparison tube.Above step adopts the method identical with solution to be measured to make the 4th blank color comparison tube, and then can ensure that the 4th blank color comparison tube adopts identical condition to make with the second color comparison tube of solution to be measured, can carry out reliable and effective contrast.
(18) standard solution of the many groups of configuration containing variable concentrations manganese dioxide is in multiple standard pipe;
(19) in above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe, add the potassium metaperiodate of weight e1 respectively;
(20) by above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe heat time e2 in boiling water bath, and stir, until each solution reaches spectrophotometric colorimetric condition, take out and be cooled to temperature b6;
(21) under the illumination of wavelength 530nm, colorimetric assay is carried out.The method is spectrophotometric method, and spectrophotometric method is absorbance by measuring measured matter light in certain wave strong point or a wavelength range or luminous intensity, this material is carried out to the method for qualitative and quantitative analysis.In spectrophotometer, when the light of different wave length is irradiated to certain density sample solution continuously, just can obtain the absorption intensity corresponding with different wave length.As with wavelength (λ) for horizontal ordinate, absorption intensity (A) is ordinate, just can draw the absorption spectrum curve of this material.Utilize this curve to carry out qualitative, the quantitative analytical approach of material, be called spectrophotometric method, also referred to as absorption spectroscopy.Measure the method for colourless substance with ultraviolet source, be called ultraviolet spectrophotometry; Measure the method for coloring matter with visible light source, be called visible ray photometry.They are the same with colourimetry, all based on Beer-Lambert law.Above-mentioned ultraviolet region and visible region are conventional.But the Ying Yongguang district of spectrophotometric method comprises ultraviolet region, visible region, infrared light district.Wavelength coverage 1) ultraviolet region of 200 ~ 400nm, 2) visible region of 400 ~ 760nm, 3) the infrared light district of 2.5 ~ 25 μm (counting 4000cm<-1> ~ 400cm<-1> by wave number).What the present invention adopted is visible region, is convenient to observe.
(22) utilize the colorimetric assay value drawing standard curve of the standard solution in each standard pipe, the colorimetric assay value then contrasted in the second color comparison tube and the 4th color comparison tube extrapolates the levels of manganese in operating environment air and mineral compound thereof.Specific formula for calculation can be: xa2d4/ d3=z;
In formula, x is the concentration that in operating environment air, manganese and mineral compound thereof are converted into manganese ion, and z is the content of solution manganese ion to be measured in the second color comparison tube;
Obtain x=(zd3)/(a2d4).
Preferably, in above-mentioned steps (2), above-mentioned first glass fiber filter paper is in the upstream of air-flow direction, and above-mentioned second glass fiber filter paper is in the downstream of air-flow direction.Due to the most of particle positively chargeds in air, therefore electronegative first glass fiber filter paper is placed on upstream, greatly can improves sampling efficiency.
Preferably, repeat corresponding steps, make many groups the second color comparison tube, extrapolate the levels of manganese in many group jobs surrounding air and mineral compound thereof, then average.Can accidental error be avoided like this, improve the accuracy of the Concentration Testing of manganese and mineral compound thereof.
In order to specifically and efficiently realize sampling and the testing process of manganese and mineral compound thereof, preferably, above-mentioned wind speed a1 is that 8-12(specifically can be 8,9,10,11 or 12) L/min; Above-mentioned volume a2 is that 800-1200(specifically can be 800,850,900,950,1000,1050,1100,1150 or 1200) L; Above-mentioned volume b1 is that 60-80(specifically can be 60,65,70,75 or 80) ml; Above-mentioned concentration b2 is that volumetric concentration 80-90(specifically can be 80,82,84,86,88 or 90) %; Above-mentioned volume b3 is that 8-12(specifically can be 8,9,10,11 or 12) ml; Said temperature b4 is that 245-250(specifically can be 245,246,247,248,249 or 250) DEG C; Above-mentioned time b5 is that 3-10(specifically can be 3,4,5,6,7,8,9 or 10) minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is that 10-30(specifically can be 10,15,20,25 or 30) mg/ml; Above-mentioned volume b8 is that 0.05-0.5(specifically can be 0.05,0.1,0.2,0.3,0.4 or 0.5) ml; Above-mentioned programming rate b9 is that 2-5(specifically can be 2,3,4 or 5) DEG C/min; Above-mentioned volume c1 is that 20-30(specifically can be 20,22,24,26,28 or 30) ml; Above-mentioned programming rate c2 is that 10-20(specifically can be 10,12,14,16,18 or 20) DEG C/min; Said temperature c3 is that 90-95(specifically can be 90,91,92,93 or 94) DEG C; Above-mentioned time c4 is that 2-3(specifically can be 2,2.2,2.4,2.6,2.8 or 3) minute; Above-mentioned volume d1 is that 40-60(specifically can be 40,45,50,55 or 60) ml; Above-mentioned volume d2 is that 4-10(specifically can be 4,5,6,7,8,9 or 10) ml; Above-mentioned volume d3 is that 40-60(specifically can be 40,45,50,55 or 60) ml; Above-mentioned volume d4 is that 20-25(specifically can be 20,21,22,23,24 or 25) ml; Above-mentioned weight e1 is that 0.25-0.3(specifically can be 0.25,0.26,0.27,0.28,0.29 or 0.3) g; Above-mentioned time e2 is 25-30 minute.
Further preferably, above-mentioned wind speed a1 is 9.5-10.5L/min; Above-mentioned volume a2 is 950-1050L; Above-mentioned volume b1 is 65-75ml; Above-mentioned concentration b2 is volumetric concentration 84-86%; Above-mentioned volume b3 is 9.5-10.5ml; Said temperature b4 is 247-248 DEG C; Above-mentioned time b5 is 5-7 minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is 15-25mg/ml; Above-mentioned volume b8 is 0.1-0.3ml; Above-mentioned programming rate b9 is 3-4 DEG C/min; Above-mentioned volume c1 is 24-26ml; Above-mentioned programming rate c2 is 14-16 DEG C/min; Said temperature c3 is 92-93 DEG C; Above-mentioned time c4 is 2.3-2.7 minute; Above-mentioned volume d1 is 45-55ml; Above-mentioned volume d2 is 6-8ml; Above-mentioned volume d3 is 45-55ml; Above-mentioned volume d4 is 22-23ml; Above-mentioned weight e1 is 0.27-0.28g; Above-mentioned time e2 is 27-28 minute.
Preferably, the aperture size of above-mentioned glass fiber filter paper is that 0.6-0.9(specifically can be 0.6,0.7,0.8 or 0.9) um.Can ensure that in operating environment air, all floating particles are all collected like this, realize effectively sampling.
Preferably, in above-mentioned steps (20), above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe are taken out after boiling water bath, before developing the color, leave standstill 1.5-2.5 hour.The solution that is detected can be made so more stable, and testing result is also more accurately reliable.
Preferably, in above-mentioned steps (20), if the solution to be measured in above-mentioned second color comparison tube is purple, dropwise instill with hydrogen peroxide, until color fade, and measure the absorbance of chromium ion, finally deduct the absorbance of chromium ion by total absorbance value, to get rid of the impact of chromium ion on testing result, improve and detect degree of accuracy.
Product form of the present invention is not limited to this case embodiment, and anyone carries out suitable change or the modification of similar thinking to it, all should be considered as not departing from patent category of the present invention.
Claims (8)
1. detect a method for manganese and mineral compound content thereof in operating environment air, it is characterized in that, comprise the steps:
(1) get glass fiber filter paper two panels, adopt friction or electron stream method of radiating to make the first glass fiber filter paper electronegative, adopt friction or positive ion stream method of radiating to make the second glass fiber filter paper positively charged;
(2) by the first glass fiber filter paper and the suction opeing of the parallel block of the second glass fiber filter paper at metering aspirator, and keep, between the first glass fiber filter paper and the second glass fiber filter paper, there is clearance for insulation;
(3) record operating environment air themperature and air pressure, open metering aspirator and sample with wind speed a1 extracting air volume a2;
(4) after sampling terminates, first glass fiber filter paper and the second glass fiber filter paper are taken off, and ensure that windward side is upward, slowly steadily put into first beaker of volume b1, ensure that the particle that the first glass fiber filter paper and the second glass fiber filter paper are adsorbed can not drop;
(5) in the first beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the first beaker is heated, and carry out stirring or shearing, the first glass fiber filter paper and the second glass fiber filter paper are dissolved completely;
(6) the first beaker is cooled to temperature b6; If now pitchy appears in solution, add the ammonium nitrate of concentration b7, volume b8, then with programming rate b9, the first beaker is heated, until yellow gas overflows completely;
(7) in the first beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted;
(8) with programming rate c2, the first beaker is heated, make the first beaker reach temperature c3 and retention time c4;
(9) with filter paper, the solution in the first beaker is filtered while keeping the first beaker temperature c3, contaminant filter is fallen, and make solution directly fall into first color comparison tube of volume d1, and with the clear water of volume d2, the first beaker, filter paper and impurity are rinsed, make washing fluid also flow in the first color comparison tube, measure overall solution volume d3;
(10) in the first color comparison tube, the solution to be measured of volume d4 is got in the second color comparison tube;
(11) the 3rd glass fiber filter paper of blank and the 4th glass fiber filter paper are put into second beaker of volume b1;
(12) in the second beaker, add the phosphoric acid of concentration b2, volume b3, with temperature b4, time b5, the second beaker is heated, and carry out stirring or shearing, the 3rd glass fiber filter paper and the 4th glass fiber filter paper are dissolved completely;
(13) the second beaker is cooled to temperature b6;
(14) in the second beaker, add the clear water of volume c1, carry out stirring simultaneously and dissolution homogeneity is diluted;
(15) with programming rate c2, the second beaker is heated, make the second beaker reach temperature c3 and retention time c4;
(16) with filter paper, the solution in the second beaker is filtered while keeping the second beaker temperature c3, contaminant filter is fallen, and make solution directly fall into the 3rd color comparison tube of volume d1, and with the clear water of volume d2, the second beaker, filter paper and impurity are rinsed, make washing fluid also flow in the 3rd color comparison tube, measure overall solution volume d3;
(17) in the solution getting volume d4 in the 3rd color comparison tube and the 4th color comparison tube;
(18) standard solution of the many groups of configuration containing variable concentrations manganese dioxide is in multiple standard pipe;
(19) in above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe, add the potassium metaperiodate of weight e1 respectively;
(20) by above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe heat time e2 in boiling water bath, and stir, until each solution reaches spectrophotometric colorimetric condition, take out and be cooled to temperature b6;
(21) under the illumination of wavelength 530nm, colorimetric assay is carried out;
(22) utilize the colorimetric assay value drawing standard curve of the standard solution in each standard pipe, the colorimetric assay value then contrasted in the second color comparison tube and the 4th color comparison tube extrapolates the levels of manganese in operating environment air and mineral compound thereof.
2. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 1, it is characterized in that: in above-mentioned steps (2), above-mentioned first glass fiber filter paper is in the upstream of air-flow direction, and above-mentioned second glass fiber filter paper is in the downstream of air-flow direction.
3. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 2, it is characterized in that: repeat corresponding steps, make many groups the second color comparison tube, extrapolate the levels of manganese in many group jobs surrounding air and mineral compound thereof, then average.
4. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 3, is characterized in that: above-mentioned wind speed a1 is 8-12L/min; Above-mentioned volume a2 is 800-1200L; Above-mentioned volume b1 is 60-80ml; Above-mentioned concentration b2 is volumetric concentration 80-90%; Above-mentioned volume b3 is 8-12ml; Said temperature b4 is 245-250 DEG C; Above-mentioned time b5 is 3-10 minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is 10-30mg/ml; Above-mentioned volume b8 is 0.05-0.5ml; Above-mentioned programming rate b9 is 2-5 DEG C/min; Above-mentioned volume c1 is 20-30ml; Above-mentioned programming rate c2 is 10-20 DEG C/min; Said temperature c3 is 90-95 DEG C; Above-mentioned time c4 is 2-3 minute; Above-mentioned volume d1 is 40-60ml; Above-mentioned volume d2 is 4-10ml; Above-mentioned volume d3 is 40-60ml; Above-mentioned volume d4 is 20-25ml; Above-mentioned weight e1 is 0.25-0.3g; Above-mentioned time e2 is 25-30 minute.
5. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 4, is characterized in that: above-mentioned wind speed a1 is 9.5-10.5L/min; Above-mentioned volume a2 is 950-1050L; Above-mentioned volume b1 is 65-75ml; Above-mentioned concentration b2 is volumetric concentration 84-86%; Above-mentioned volume b3 is 9.5-10.5ml; Said temperature b4 is 247-248 DEG C; Above-mentioned time b5 is 5-7 minute; Said temperature b6 is room temperature; Above-mentioned concentration b7 is 15-25mg/ml; Above-mentioned volume b8 is 0.1-0.3ml; Above-mentioned programming rate b9 is 3-4 DEG C/min; Above-mentioned volume c1 is 24-26ml; Above-mentioned programming rate c2 is 14-16 DEG C/min; Said temperature c3 is 92-93 DEG C; Above-mentioned time c4 is 2.3-2.7 minute; Above-mentioned volume d1 is 45-55ml; Above-mentioned volume d2 is 6-8ml; Above-mentioned volume d3 is 45-55ml; Above-mentioned volume d4 is 22-23ml; Above-mentioned weight e1 is 0.27-0.28g; Above-mentioned time e2 is 27-28 minute.
6. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to any one of claim 1-5, is characterized in that: the aperture size of above-mentioned glass fiber filter paper is 0.6-0.9um.
7. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 6, it is characterized in that: in above-mentioned steps (20), above-mentioned second color comparison tube, the 4th color comparison tube and each standard pipe are taken out after boiling water bath, before developing the color, leave standstill 1.5-2.5 hour.
8. a kind of method detecting manganese and mineral compound content thereof in operating environment air according to claim 6, it is characterized in that: in above-mentioned steps (20), if the solution to be measured in above-mentioned second color comparison tube is purple, dropwise instill with hydrogen peroxide, until color fade, and measure the absorbance of chromium ion, finally deduct the absorbance of chromium ion by total absorbance value, to get rid of the impact of chromium ion on testing result.
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| CN106770262A (en) * | 2017-02-22 | 2017-05-31 | 济宁利特纳米技术有限责任公司 | A kind of method of graphene oxide powder manganese content detection |
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| SU1019298A1 (en) * | 1981-10-28 | 1983-05-23 | Всесоюзный научно-исследовательский институт техники безопасности в химической промышленности | Indicator compound for qualitative determination of chlorbenzene in air |
| CN103389299A (en) * | 2013-06-26 | 2013-11-13 | 天津虹炎科技有限公司 | Content measurement of manganese element in environment based on ICP method |
| CN104215595A (en) * | 2014-09-17 | 2014-12-17 | 陕西华陆化工环保有限公司 | Method for detecting trace manganese in environmental sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| SU1019298A1 (en) * | 1981-10-28 | 1983-05-23 | Всесоюзный научно-исследовательский институт техники безопасности в химической промышленности | Indicator compound for qualitative determination of chlorbenzene in air |
| CN103389299A (en) * | 2013-06-26 | 2013-11-13 | 天津虹炎科技有限公司 | Content measurement of manganese element in environment based on ICP method |
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| CN106770262A (en) * | 2017-02-22 | 2017-05-31 | 济宁利特纳米技术有限责任公司 | A kind of method of graphene oxide powder manganese content detection |
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Denomination of invention: Method for detecting manganese and manganese inorganic compounds in air of operation environment Effective date of registration: 20200519 Granted publication date: 20160824 Pledgee: Agricultural Bank of China Limited Fuzhou Taijiang sub branch Pledgor: FUJIAN TUOPU DETECTION TECHNOLOGY Co.,Ltd. Registration number: Y2020350000034 |