CN101975714B - Method for measuring adsorption quantity of fatty acid collector on mineral surface - Google Patents
Method for measuring adsorption quantity of fatty acid collector on mineral surface Download PDFInfo
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Abstract
The invention relates to a method for measuring the adsorption quantity of a fatty acid collector on a mineral surface, which is characterized by comprising the following steps of: 1) measuring a concentration value of a produced carbon dioxide gas by using a constant volume combustion fatty acid collector, and recording an average concentration value of the carbon dioxide gas; and 2) calculating the adsorption quantity of the fatty acid collector on the mineral surface by the conventional method according to the average concentration value of the carbon dioxide gas. The concentration of a detected gas in combustion gases is improved by the constant volume combustion method and the sensitivity and speed of detecting the adsorption quantity of the fatty acid collector on the mineral surface by the combustion method are improved.
Description
Technical field
The present invention relates to the assay method of a kind of fatty acid collecting agent in the mineral surface adsorbance.
Background technology
Although constantly have new technique of preparing and technology to emerge in large numbers and use, remain floatation as the main force of ore dressing.The factor that influences flotation is a lot, still is floating agent mainly, and wherein most important is exactly flotation collector.The main effect of collecting agent promptly is to be adsorbed on the purpose mineral for the treatment of flotation selectively and to make it hydrophobic.One, collecting agent will directly determine flotation results in the absorption and the distribution situation of mineral surface.To understanding in depth of this process, unusual meaning is all arranged to understanding floatation process and finding out the approach that improves floatation indicators, reduces reagent consumption.Therefore, in flotation research, just seem extremely important in the research of absorption mechanism on the purpose mineral and adsorbance about collecting agent.
Assay method about the flotation collector adsorbance can be divided into two kinds: direct method and indirect method.Direct method promptly is directly to measure the concentration of collecting agent on mineral surface.This can be divided into in-site detecting method (in-situ measurement) and dystopy determination method (ex-situ measurement) again.In-site detecting promptly is the liquid-solid interface in collecting agent and mineral effect, under the promptly real flotation pulp condition, measures the concentration of collecting agent on mineral surface.Dystopy measure promptly be with the collecting agent effect after mineral grain from liquid phase, separate, in gas phase or vacuum, measure the concentration of collecting agent on mineral surface again.Although in-site detecting more can reflect the reality of flotation system, can accomplish that the method for in-site detecting is also few, as ATR-IR, laser Raman spectroscopy etc.; Majority method remains the dystopy assay method, as FTIR, XPS, ToF-SIMS etc.
The indirect determination method promptly is the variation by collecting agent concentration in the liquid phase before and after mensuration and the mineral effect, maybe will be adsorbed with the mineral grain and the liquid phase separation of collecting agent, thereby and then extrapolate the concentration of collecting agent on mineral surface indirectly with the concentration that solvent is measured collecting agent in the stripping liquid after with the quantitative desorb of these collecting agents that are adsorbed, enrichment again.The indirect determination method is not because there is the interference of mineral grain, and chemical analysis method applicatory is a lot, as FTIR, DRIFT-FTIR, ultraviolet spectrum etc., so be the most frequently used adsorption of collector quantity measuring method.
Is the comparison difficulty to collecting agent in the flotation in the research of mineral surface absorption, and this is because collecting agent occurs over just in the mineral surface layer in the absorption of mineral surface.The thickness of superficial layer one in several nanometers between tens nanometers.This size is not in the resolution scope of optical microscope or even electron microscope.The volume ratio that the volume of superficial layer accounts for whole solid phase also is very small.Analyze the adsorption of collector amount in so few superficial layer, just need a large amount of superficial layers for analyzing.The fatty acid commonly used with oxide ore flotation is example, by a fatty acid molecule at the area that mineral surface absorption is covered is
Meter is 1m as the mineral specific surface area
2/ g (this is a very high default for most of ore dressing systems) forms complete unimolecular layer cover cap when fatty acid restrains one so on such sample, the fatty acid amount that it contained also only is 8.3 * 10
-6Mole.So low content has exceeded the sensing range of most of analytical approachs.Traditional analysis fatty-acid collector draws with analyses such as spectrophotometric method after the solvent evaporated after the method for mineral surface adsorbance is to extract with volatile solvent (as chloroform) again.For the fatty acid of chemisorption on the phosphate surface, have data think solvent extraction process difficulty reach balance.And for a large amount of fine-graded materials are arranged, the separation of extraction back phase can be compared difficulty again.Thereby particularly will be very difficult to the mensuration of the adsorption of collector amount of the material behind the fine grinding ore deposit to actual sample ore.On the other hand, will use a large amount of extractants to the toxic effect of human body in the extraction process, this is environmental protection neither, has also increased analysis cost.
It is a kind of fairly simple and practical method in the adsorbance of mineral surface that firing method is measured fatty acid collecting agent.The principle of this method is: will be adsorbed with sample fully burning under suitable temperature of fatty acid collecting agent, analyze the amount of the carbon dioxide in the gas that is produced then, thus the counter amount of releasing the adsorbed collecting agent of sample.This method still belongs to direct assay method in essence, and it is to be founded in 1962 by the Balint of London University the earliest, after Howe
[1～2], Pugh
[5]And Miettinen
[6]Improve the back and be tending towards ripe and practical gradually Deng the people.Also derive some other similar method thus, as HAGIS
[7～8]Method.The flotation system of using this method research has fluorite, apatite and galenite etc.
Howe
[1～4]Deng method be with not with the sample ore of collecting agent effect as the reference sample, be adsorbed with the sample ore of collecting agent and the heat difference that the reference sample ore is discharged with the DTA methods analyst in the heating flame process, calculate the amount (the burning thermal discharge is directly proportional with the amount of the collecting agent of mineral surface) of the collecting agent of mineral surface absorption by the heat difference that discharges.It is said that the fatty acid adsorbance of measuring mineral surface in this way can reach 0.1mg/g, promptly ten thousand/ detectability.
Pugh
[5]Method with above-mentioned different.As shown in Figure 1, it is that the sample ore that will be adsorbed with collecting agent burns in first stove earlier in pure oxygen atmosphere, enter the clean-burning catalyzing carbon monoxide that do not have that second stove will produce subsequently and be converted into carbon dioxide, surveying the gas concentration lwevel of discharging in the gas with highly sensitive carbon dioxide detector at last, promptly is the total carbon dioxide capacity that sample combustion discharged according to gas concentration lwevel * flow to the integration of time.Be limited to 20 μ g/m under the detection of this method
2Mineral surface (in pure carbon).If the specific surface area by mineral grain is 1m
2/ g, converting is that fatty acid (oleic acid) is measured, its detectability is roughly in 26 μ g/g levels, promptly roughly in 100,000/level.A lot of TOC and elemental analyser promptly are this test modes that adopts.
Miettinen
[6]Etc. used apparatus is to form through necessary transformation on commerical grade Combustion tester LECO RC-412, as shown in Figure 2.The burning carrier gas is promptly gone into combustion chambers burn after being further purified (removing organism, water vapour), enter sensing chamber subsequently and detect gas concentration lwevel, also detects the concentration of water vapour simultaneously.As producing simultaneously carbon dioxide and water vapor concentration peak are arranged, then showing has organic carbon to exist in the sample.The detectability of this method is roughly at 10-30g/t, and promptly the method with Pugh etc. is suitable.The maximum characteristics of this method are that it can distinguish organic carbon (collecting agent) and inorganic carbon (carbonate mineral) (judging by having or not the water vapor concentration peak).
Vreugdenhil
[7～8]Deng method--head space gas phase infrared analysis (the Headspace analysis by gas-phase infrared spectroscopy that will be in the infrared analysis analyzes volatile components, HAGIS) be incorporated into the mensuration of flotation collector adsorbance, studied the adsorbance of xanthate class collecting agent on the sulphide ore surface.As shown in Figure 3, its principle is a directly heating and decomposition in the infrared detection chamber of sample, and the gas concentration of decomposition is directly by infrared spectrum measurement.Because its infrared analysis chamber is very little, and is heating and decomposition near vacuum or nitrogen, so be unburnt thermal decomposition.So different with firing method, gas concentration lwevel and collecting agent concentration are not had a linear corresponding relation in its pyrolysis product, be between the COS of one of xanthate pyrolysis product and xanthate concentration good corresponding relation to be arranged on the contrary.This method may be inapplicable to the mensuration of fatty acid collecting agent, because simple thermal decomposition and the gas concentration lwevel of fatty acid collecting agent do not have corresponding relation with this understanding yet.In strong well-oxygenated environment, the xanthate of sulphide ore and its surface adsorption, black powder etc. all are easy to oxidation, cause detection signal not to be easily distinguishable.Unique advantage of this method is in very low collector dosage scope, and detection signal also has good linear corresponding relation with collecting agent concentration.So it is suitable for the analysis and research of the relatively low sulfide mineral collector of collector dosage very much.
By above literature review as seen, existing combustion analysis method majority is combustion analysis in carrier gas.For guaranteeing that sample fully burns, need to keep carrier gas that certain pressure and flow are arranged.When analyzing small amount of sample, bigger carrier gas stream can reduce the concentration of the object gas (as carbon dioxide) in the analytical gas virtually.This is that above analytical approach detection limit is than higher basic reason.Simultaneously bigger current-carrying is also had higher requirement to detecting detector sensitivity, thus will be with the detecting device of high sensitivity, and instrument is comparatively valuable.Though the HAGIS method is without carrier gas, as preceding analysis, directly heating is a Non-oxygen pyrolytic in sensing chamber, to the mensuration of fatty acid collecting agent and inapplicable.In addition, its heating element also can produce infrared radiation and may produce interference to infrared detection device.
List of references
[1]T.M.Howe，M.I.Pope.The?quantitative?determination?of?flotation?agentsadsorbed?on?mineral?powders?using?differential?Thermal?analysis[J].PowderTechnology.1970/71，(4)：338-344.
[2]M.I.Pope，D.I.Sutton.The?correlation?between?froth?flotation?responseand?collector?adsorption?from?aqueous?solution.Part?I.Titanium?dioxide?and?ferricoxide?conditioned?in?oleate?solutions[J].Powder?Technology.1973，(7)：271-279.
[3]M.I.Pope，D.I.Sutton.The?correlation?between?froth?flotation?responseand?collector?adsorption?from?aqueous?solution.Part?II.Titanium?dioxide?and?ferricoxide?conditioned?in?n-dodecylamine?solutions[J].Powder?Technology.1974，(9)：273-277.
[4]M.I.Pope，D.I.Sutton.The?correlation?between?froth?flotation?responseand?collector?adsorption?from?aqueous?solution.Part?III.Water?vapour?adsorptionon?titanium?dioxide?conditioned?in?n-dodecylamine?solutions[J].Powder?Technology.1974，(10)：251-255.
[5]R.J.Pugh，K.Husby.Qantitative?determination?of?col?lector?adsorbed?onfluorite，galena，and?quartz?particles?by?selective?oxidation?surface?analysis[J].International?Journal?of?Mineral?Processing，1986，18(3-4)：263-275.
[6]M.Miettinen，P.Stén，S.
J.Leppinen，J.Aaltonen.Determinationof?chemicais?bound?to?mineral?surfaces?in?flotation?processes[J].MineralsEngineering，2000，13(3)：245-254.
[7]A.J.Vreugdenhil，J.A.Finch，I.S.Butler，I.Paquin.Analysis?ofalkylxanthate?collectors?on?sulphide?minerals?and?flotation?products?by?haedspaceanalysis?gas-phase?infrared?spectroscopy(HAGIS)[J].Minerals?Engineering，1999，12(7)：745-756.
[8]D.Lascelles，J.A.Finch.A?technique?for?quantification?of?adsorbedcollectors：xanthate[J].Minerals?Engineering，2005，18(2)：257-262.
Though there are a lot of modern measuring technologies can be used for measuring the adsorbance of fatty acid collecting agent at mineral surface, sensitive, convenient and practical method is also few.
Summary of the invention
The object of the present invention is to provide the assay method of a kind of fatty acid collecting agent easily, this method detection sensitivity height in the mineral surface adsorbance.
For achieving the above object, the technical solution used in the present invention is: a kind of fatty acid collecting agent is at the assay method of mineral surface adsorbance, it is characterized in that it comprises the steps: 1) employing constant volume combustion fatty acid collecting agent, measure the concentration value of the carbon dioxide that is produced, write down the mean intensity value of carbon dioxide; 2) according to the mean intensity value of carbon dioxide, convert out fatty acid collecting agent in the mineral surface adsorbance by existing conventional method.
Described step 1) is specially:
1. measurement mechanism: measurement mechanism comprises welding bottle 1, first pipeline 4, first solenoid valve 5, second pipeline 6, second solenoid valve 7, catalytic combustion burner 8, the 3rd pipeline 9, CO
2Display instrument 10, the 4th pipeline 11, computing machine 12, peristaltic pump 13, gas concentration sensor 14, container 15, sample combustion stove 16, the 5th pipeline 17, the 3rd solenoid valve 18, one end of first pipeline 4 links to each other with the output port of welding bottle 1, the other end of first pipeline 4 is connected with first port of catalytic combustion burner 8, and first pipeline 4 is provided with first solenoid valve 5; Second port of catalytic combustion burner 8 is connected by first port of the 3rd pipeline 9 with the container 15 of sealing, be provided with 2 gas concentration sensors 14 in the container 15, be respectively the gas concentration sensor that is used to measure density of carbon dioxide gas, the gas concentration sensor that is used to measure carbon monoxide gas concentration, the signal output part of gas concentration sensor 14 by signal wire respectively with CO
2The signal input part of the signal input part of display instrument 10, computing machine 12 links to each other; One end of the 4th pipeline 11 is connected with second port of container 15, and the other end of the 4th pipeline 11 is connected with first port of sample combustion stove 16, and the 4th pipeline 11 is provided with peristaltic pump 13; One end of the 5th pipeline 17 is connected with second port of sample combustion stove 16, and the other end of the 5th pipeline 17 is the emptying end, and the 5th pipeline 17 is provided with the 3rd solenoid valve 18; One end of second pipeline 6 is connected with first pipeline 4 by three-way connection, and an end of second pipeline 6 is between first solenoid valve 5 and catalytic combustion burner 8, the other end of second pipeline 6 is connected with the 5th pipeline 17 by three-way connection, and the other end of second pipeline 6 is between the 3rd solenoid valve 18 and sample combustion stove 16;
2. earlier the load weighted sample that contains fatty acid collecting agent is packed in the sample combustion stove 16, catalyzer is put into catalytic combustion burner 8, open first solenoid valve 5, the 3rd solenoid valve 18, close second solenoid valve 7, catalytic combustion burner 8 is warming up to 600 ℃, open the oxygen cylinder valve 2 on the welding bottle 1, open peristaltic pump 13 then, high purity oxygen gas in the welding bottle 1 is with first pipeline 4, catalytic combustion burner 8, the 3rd pipeline 9, container 15, the 4th pipeline 11, peristaltic pump 13, sample combustion stove 16 and the 5th pipeline 17 hollow gas drives are caught up with and are done to the greatest extent, and are full of oxygen to 1～1.1atm pressure; Close the oxygen cylinder valve 2 on the welding bottle 1 then, close first solenoid valve 5, the 3rd solenoid valve 18, open second solenoid valve 7, sample combustion stove 16 begins to heat up, sample combustion stove 16 is heated the fatty acid collecting agent sample, and fatty acid collecting agent and oxygen reaction generate CO in the time of 400～500 ℃
2And CO, catalyzer is CO with the CO catalytic oxidation
2The concentration of while opening entry carbon dioxide, CO gas; After the furnace temperature of sample combustion stove 16 reaches 400～500 ℃ of the temperature that set, keep furnace temperature, write down the mean intensity value of carbon dioxide, CO gas.
The invention has the beneficial effects as follows: the present invention is mainly reflected in combustion system and changes into closed circuit by traditional open circuit, adopt constant volume combustion method to improve the concentration of detected gas in the burning gases, measure detection sensitivity and the detection speed of fatty acid collecting agent in the mineral surface adsorbance thereby improved firing method.The present invention is a kind of constant volume, pressure oxygen round-robin burning determination method, compares with the traditional combustion method, and this subtraction unit is simpler, easier realization, and detection sensitivity height, accurately.
Description of drawings
Fig. 1 is a Pugh analysis of experiments general flow chart.
Fig. 2 is a Miettinen analysis of experiments general flow chart.
Fig. 3 is a Vreugdenhil test unit sketch; Among Fig. 3: (a) stainless steel example boat, (b) with the Teflon plug of dismountable KRS-window, (c) attemperating unit, (d) vacuum switch plug.
Fig. 4 is the structural representation of the device (abbreviation measurement mechanism) of measurement fatty acid collecting agent adsorbance; Among Fig. 4: 1-welding bottle, 2-oxygen cylinder valve, 3-rain glass, 4-first pipeline, 5-first solenoid valve (first switch), 6-second pipeline, 7-second solenoid valve (second switch), 8-catalytic combustion burner, 9-the 3rd pipeline, 10-CO
2Display instrument (device), 11-the 4th pipeline, 12-computing machine (record CO
2Concentration), 13-peristaltic pump, 14-gas concentration sensor, 15-container, 16-sample combustion stove, 17-the 5th pipeline, 18-the 3rd solenoid valve (the 3rd switch).
Fig. 5 is typical CO
2Test curve figure.
Embodiment
A kind of fatty acid collecting agent is at the assay method of mineral surface adsorbance, and it comprises the steps:
1) adopts the constant volume combustion fatty acid collecting agent, measure the concentration value of the carbon dioxide that is produced, write down the mean intensity value (being closed circuit measurement) of carbon dioxide; Be specially:
1. the preparation of measurement mechanism: as shown in Figure 4, measurement mechanism comprises welding bottle 1, first pipeline 4, first solenoid valve 5, second pipeline 6, second solenoid valve 7, catalytic combustion burner 8, the 3rd pipeline 9, CO
2Display instrument (or claiming carbon dioxide to detect display instrument) the 10, the 4th pipeline 11, computing machine 12, peristaltic pump 13, gas concentration sensor 14, container 15, sample combustion stove 16, the 5th pipeline 17, the 3rd solenoid valve 18, one end of first pipeline 4 links to each other with the output port of welding bottle 1, the other end of first pipeline 4 is connected with first port of catalytic combustion burner 8, and first pipeline 4 is provided with first solenoid valve 5; Second port of catalytic combustion burner 8 is connected by first port of the 3rd pipeline 9 with the container 15 of sealing (sealing), be provided with 2 gas concentration sensors 14 in the container 15, be respectively the gas concentration sensor that is used to measure density of carbon dioxide gas, the gas concentration sensor that is used to measure carbon monoxide gas concentration, the signal output part of gas concentration sensor 14 by signal wire (data line) respectively with CO
2The signal input part of the signal input part of display instrument 10, computing machine 12 links to each other; One end of the 4th pipeline 11 is connected with second port of container 15, and the other end of the 4th pipeline 11 is connected with first port of sample combustion stove 16, and the 4th pipeline 11 is provided with peristaltic pump 13; One end of the 5th pipeline 17 is connected with second port of sample combustion stove 16, and the other end of the 5th pipeline 17 is the emptying end, and the 5th pipeline 17 is provided with the 3rd solenoid valve 18; One end of second pipeline 6 is connected with first pipeline 4 by three-way connection, and an end of second pipeline 6 is between first solenoid valve 5 and catalytic combustion burner 8, the other end of second pipeline 6 is connected with the 5th pipeline 17 by three-way connection, and the other end of second pipeline 6 is between the 3rd solenoid valve 18 and sample combustion stove 16; Catalytic combustion burner 8, sample combustion stove 16 have temperature controller respectively; First pipeline 4 is provided with rain glass 3;
2. will load weightedly be adsorbed with earlier in sample [sample of the fatty acids collecting agent of the present embodiment employing 1g] sample combustion of packing into the stove 16 of fatty acid collecting agent, catalyzer is put into catalytic combustion burner 8, and (present embodiment adopts 100g, catalyzer adopts CuO and MnO potpourri, the mass ratio of CuO and MnO is: 6: 4), open first solenoid valve 5, the 3rd solenoid valve 18, close second solenoid valve 7, catalytic combustion burner 8 is warming up to 600 ℃, and (600 ℃ is the minimum temperature requirement, can be higher, react faster, but require also high to reacting furnace), open the oxygen cylinder valve 2 on the welding bottle 1, open peristaltic pump 13 then, (described high purity oxygen gas is a purity 〉=99.999v/v%) with first pipeline 4 to high purity oxygen gas in the welding bottle 1, catalytic combustion burner 8, the 3rd pipeline 9, container 15, the 4th pipeline 11, peristaltic pump 13, sample combustion stove 16 and the 5th pipeline 17 hollow gas drives are caught up with and are done (detecting device makes zero) to the greatest extent, and be full of oxygen to 1～1.1atm pressure (a little more than 1atm, the water column pressure measurement), the reading of carbon dioxide and carbon monoxide is zero at this moment; Close the oxygen cylinder valve 2 (promptly closing source of oxygen) on the welding bottle 1 then, close first solenoid valve 5, the 3rd solenoid valve 18, open second solenoid valve 7, sample combustion stove 16 begins to heat up, sample combustion stove 16 is heated the fatty acid collecting agent sample, and fatty acid collecting agent and oxygen reaction generate CO in the time of 400～500 ℃
2And CO, catalyzer is CO with the CO catalytic oxidation
2(peristaltic pump 13 makes gas circulation and mixes); The concentration of while opening entry carbon dioxide, CO gas; After the furnace temperature of sample combustion stove 16 reaches 400～500 ℃ of the temperature that set, keep furnace temperature, (the carbon monoxide reading is nonsensical, and it just is used to monitor, and catalyzing carbon monoxide transforms fully, reaction fully promptly reaches terminal point to write down the mean intensity value (final equilibrium value) of carbon dioxide, CO gas.The carbon monoxide reading value can make zero again because of it all is converted into carbon dioxide).Typical test results (CO
2) as shown in Figure 5.
2) according to the mean intensity value of carbon dioxide, [conversion is corresponding fatty acid amount in the mineral surface adsorbance to convert out fatty acid collecting agent by existing conventional method.Can calculate with theoretical value or formula.Commonly used is to proofread and correct with standard substance, and correction work is complicated slightly, be proofreaied and correct by two steps and finish.Need the school carbon dioxide sensor earlier: find out the linear relationship between amount of carbon dioxide and sensor reading with calcium oxalate thermal decomposition (500 ℃), demarcate the amount of carbon dioxide of the reading representative of carbon dioxide sensor; Second step be the amount of demarcating fatty acid collecting agent with the carbon dioxide of its burning generation between linear relationship; Fatty acid collecting agent promptly is the adsorbed collecting dosage of unit mass mineral in the mineral surface adsorbance, and the fatty acid amount that promptly records is removed sample (being mineral) quality and is adsorbance].
Because the volume of whole analysis system is (constant volume) fixed, when the detectability of gas concentration sensor 14 between 0.1～1ppm when (is example with the carbon dioxide), volume as system is 2 liters, and the carbon dioxide absolute magnitude of whole system is 0.00036～0.0036mg.As sampling amount is 1g, and then the detection limit of this method is roughly at 0.00036～0.0036mg/g, i.e. 0.36～3.6 μ g/g (anthracometer).Be about for corresponding fatty acid amount (oleic acid) as conversion: 0.14～1.4 μ g/g.This lower limit approximately can reduce one to two order of magnitude than existing method, promptly is easy to reach 1,000,000/ detection levels to 1/10000000th, and this is minimum in all methods up to now.Illustrate that the present invention has improved firing method and measured detection sensitivity and the detection speed of fatty acid collecting agent in the mineral surface adsorbance.Obviously, as design sample porcelain boat volume containing the sample big again (as being 10 to restrain), the system volume further reduces again or adopt more sensitive detecting sensor, the analysis lower limit of the method order of magnitude that also is expected to descend again.
Because the fatty acid amount of analyzing is few, so the combustion process oxygen consumption is few, organic in addition burning does not increase the gas phase total mole number of system, does not promptly increase the volume of system.The volumetric expansion that the variation of system volume is mainly heated and caused by gas phase.When gases are heated, they expand owing to have only in the heating tube part, so the variation of whole system pressure is not (by heating to 600 ℃) very greatly, still in controlled range.
Obviously, this method also can be used for the analysis of other solids or fluid sample incendivity composition, analyzes as TOC.
Claims (1)
1. a fatty acid collecting agent is at the assay method of mineral surface adsorbance, it is characterized in that it comprises the steps: 1) employing constant volume combustion fatty acid collecting agent, measure the concentration value of the carbon dioxide that is produced, write down the mean intensity value of carbon dioxide; 2) according to the mean intensity value of carbon dioxide, convert out fatty acid collecting agent in the mineral surface adsorbance by existing conventional method;
Described step 1) is specially:
1. measurement mechanism: measurement mechanism comprises welding bottle (1), first pipeline (4), first solenoid valve (5), second pipeline (6), second solenoid valve (7), catalytic combustion burner (8), the 3rd pipeline (9), CO
2Display instrument (10), the 4th pipeline (11), computing machine (12), peristaltic pump (13), gas concentration sensor (14), container (15), sample combustion stove (16), the 5th pipeline (17), the 3rd solenoid valve (18), one end of first pipeline (4) links to each other with the output port of welding bottle (1), the other end of first pipeline (4) is connected with first port of catalytic combustion burner (8), and first pipeline (4) is provided with first solenoid valve (5); Second port of catalytic combustion burner (8) is connected by first port of the 3rd pipeline (9) with the container (15) of sealing, be provided with 2 gas concentration sensors (14) in the container (15), be respectively the gas concentration sensor that is used to measure density of carbon dioxide gas, the gas concentration sensor that is used to measure carbon monoxide gas concentration, the signal output part of gas concentration sensor (14) by signal wire respectively with CO
2The signal input part of the signal input part of display instrument (10), computing machine (12) links to each other; One end of the 4th pipeline (11) is connected with second port of container (15), and the other end of the 4th pipeline (11) is connected with first port of sample combustion stove (16), and the 4th pipeline (11) is provided with peristaltic pump (13); One end of the 5th pipeline (17) is connected with second port of sample combustion stove (16), and the other end of the 5th pipeline (17) is the emptying end, and the 5th pipeline (17) is provided with the 3rd solenoid valve (18); One end of second pipeline (6) is connected with first pipeline (4) by three-way connection, and an end of second pipeline (6) is positioned between first solenoid valve (5) and the catalytic combustion burner (8), the other end of second pipeline (6) is connected with the 5th pipeline (17) by three-way connection, and the other end of second pipeline (6) is positioned between the 3rd solenoid valve (18) and the sample combustion stove (16);
2. earlier the load weighted sample that contains fatty acid collecting agent is packed in the sample combustion stove (16), catalyzer is put into catalytic combustion burner (8), open first solenoid valve (5), the 3rd solenoid valve (18), close second solenoid valve (7), catalytic combustion burner (8) is warming up to 600 ℃, open the oxygen cylinder valve (2) on the welding bottle (1), open peristaltic pump (13) then, high purity oxygen gas in the welding bottle (1) is with first pipeline (4), catalytic combustion burner (8), the 3rd pipeline (9), container (15), the 4th pipeline (11), peristaltic pump (13), sample combustion stove (16) and the 5th pipeline (17) hollow gas drive are caught up with and are done to the greatest extent, and are full of oxygen to 1～1.1atm pressure; Close the oxygen cylinder valve (2) on the welding bottle (1) then, close first solenoid valve (5), the 3rd solenoid valve (18), open second solenoid valve (7), sample combustion stove (16) begins to heat up, the sample that sample combustion stove (16) will contain fatty acid collecting agent is heated, and fatty acid collecting agent and oxygen reaction generate CO in the time of 400～500 ℃
2And CO, catalyzer is CO with the CO catalytic oxidation
2The concentration of while opening entry carbon dioxide, CO gas; After the furnace temperature of sample combustion stove (16) reaches 400～500 ℃ of the temperature that set, keep furnace temperature, write down the mean intensity value of carbon dioxide.
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| BRPI0705593B1 (en) * | 2007-11-22 | 2016-04-12 | Univ Minas Gerais | method of quantifying amines in iron ore flotation waste |
| CN101264465B (en) * | 2008-05-12 | 2011-06-08 | 昆明理工大学 | Singleness siderite full flotation ore dressing method |
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2010
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