• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A two-flame burner is used in a flame photometric detector for analyzing a sample material. The sample material is introduced via a first conduit structure into a hydrogen-rich first flame, and the combustion products and excess hydrogen from the first flame are passed via a second conduit structure into an oxygen-containing environment. A second flame is maintained at the exit end of the second conduit structure. The first and second conduit structures are composed of material that does not contribute to the coloration of the second flame during operation of the detector. Particular constituents of the sample material are detected by observing the presence of colors in the second flame indicative of the constituents. For example, the presence of sulfur is indicated by a blue coloration, and the presence of phosphorus is indicated by a green coloration. The presence of nitrogen is indicated by a coloration of the second flame resulting from a chemiluminescent molecular recombination of nitric oxide and oxygen atoms to form nitrogen dioxide molecules. The presence of any hydrocarbon can be indicated by a flame coloration resulting from a chemical reaction indicative of elemental carbon.
    公开号:SU828985A3
    申请号:SU782587044
    申请日:1978-02-27
    公开日:1981-05-07
    发明作者:Луис Пэттерсон Пол
    申请人:Вариан Ассошиэйтс Инк (Фирма)；
    IPC主号:
    专利说明:

    but with a gas chromatographic column, it is also necessary to pay attention to the fact that the chemical compounds in the effluent source 1 of the gas chromatograph are often very complex molecules. When a torch enters the environment, such molecules can disturb the temperature gradients and substances in the torch, which will have an adverse effect on the creation of light of the desired color.
    Most applications of flare photometric indicators with gas chromatographs before (Present time was intended to selectively detect only sulfur-containing or phosphorus-containing chemical compounds. If the sulfur-containing molecule is introduced into the hydrogen-rich torch of Hj mixture with 02 or with air, This characteristic blue radiation can be attributed to the excitation of the So molecule. Although the chemical mechanisms of the formation of the Sj molecule, IOLNEEEO did not confirm, kinematic and The following results suggest that sulfur-containing chemical compounds collide with the radicals H, OH and /, or O in the plume so that H2S is obtained as the head of the combustion product. H2 then turns into -3 DL with the help of new reactions , such as
    HaS + H - H + H, SH + H S + But
    SH + S - S2 + li
    After that, the S molecule is excited and then relaxed to give a characteristic blue radiation of an emitter and a chemical reaction like:
    H N - Sv S, + H2.
     When blue sulfur radiation is formed, radical N. is necessary.
    If a molecule containing phosphorus is introduced into the hydrogen-rich torch of the H2 mixture with 02 or with air, green radiation is noted. This characteristic green radiation can be attributed to the NRA molecule. Although the chemical mechanisms for the formation of an NRA molecule are not exactly confirmed, kinetic studies make it possible to suggest that phosphorus-containing compounds of nrn collisions with the H, OH and O radicals in the plume decay in such a way that the radical PO is obtained as the main combustion product. Two different materials have been proposed for the formation of an excited NRA molecule.
    H - RO + M NRA + M,
    where M is some other chemical compound; or
    OH - f PO + H2 NRA + N.O.
    The formation of green phosphorus radiation requires radicals H and OH.
    An old burner that uses a single hydrogen-rich torch both to decompose chemical compounds in the outflow of a gas chromatographic column and to create the required blue or green color indicating euir or phosphorus, respectively. The optimized velocities and currents of gases, the shape of the burner, are such that the billowing light from hydrocarbons appears at the base of the plume in close proximity to the vicinity; to the burner holes, while sulfur and phosphorus emissions appear in the scattered upper parts of the flame. These torch tops are observed with a photomultiplier tube. Selectivity is enhanced by the use of neurospray; a screen mounted next to the base of the flare in order to prevent the field of the photoelectron electronic detector 1 from reaching the field of hydrocarbon radiation.
    The limitations of such a burner are known to include the use of an elastic plume in it and the environmental disturbance of this torch caused by the southern molecular structures that are present in the gas through the chromatographic stream. Such translucent plumes can alter the sensitivity of a sample, depending on the structure of the sample molecules, as well as suppressing the sensitivity of the ipsa npsi and the simultaneous presence of a hydrocarbon fune. In addition, irn of large quantities of hydrocarbon compounds, the torch can be aspirated, as often occurs with solvents commonly used in a gas chromatograph. Moreover, due to the use of the burner-rich flame in such a mud, the gaseous products of combustion contain large excess of non-combustible Ns, which create a notional safety hazard.
    Also known is the van der Sm11ssen burner, which is intended for the spatial separation of various areas of chemical reactions of a torch burning in ambient air by means of an optically transparent tube.
    A mixture of air and a stream of flow from the chromatographic column is introduced into the tube with an even hole. The tube is oithically transparent in the visible region of the electromagnetic spectrum and is made of quartz or glass. Gaseous hydrogen is introduced into this pipe through a conduit. During operation, a hydrogen-rich first flame is ignited near the tip of another conduit inside the tube. The gaseous products burned from this first torch exited into the:: ru ;; fuse air at the top of the tube, where an excess of J-b, which was not consumed in the first torch, burns in the second torch near the Perkhm tube tip. In order to start work, the second torch is first lit. Owing to laughing No; 1; air upstream in the tube n due to the even opening of this tube, the upper torch (i.e., the second torch) causes flame to flash, which ignites the lower torch (i.e., the first srakel). Due to the fact that the upper and lower flares create high temperatures, for cooling the tube; in order to prevent excessive heated walls of quartz or Pyrex glass, in the area between the flares a water jacket is used. In the absence of sulfur and phosphorus, the lower torch has a bluish-white color, and the upper torch has a bluish, reddish or yellowish color. Since it is well known that a flame from a pure mixture of O and O, or with air, usually triggers an invisible light, painted on the upper and lower flames, probably due to impurities in the gases of their hot tips made of quartz and glass.
    In those cases when chemical compounds containing sulfur and phosphorus are present in the outflowing columns of the column, diffuse bands of blue and / or green color occur inside the tube between the lower and upper torches. The blue tip indicates the presence of sulfur-containing constituents, and the green bar indicates the presence of phosphorus-containing components. Under conditions of optimized fluxes, a green band appears in an area that is spatially closer to the lower torch than an area in which but the blue nose is. Blue radiation can be attributed to the excitation of So molecules created by the results of various chemical reactions occurring in the lower torch, and the green band can be attributed to the excitation of NRO molecules also generated by chemical reactions occurring in the lower torch. Of course, these molecules 82 and the NRA are excited again when they enter the upper torch as they exit the tube. In cases where sulfur and / or phosphorus containing elements are present in the stream, at the core of the upper flare 1 there are characteristic blue and / or green radiation. However, in accordance with the Van der Smissen method, the presence of such characteristic bare and / or green radiations is detected in the usual case by means of optical observation of a region spread in the tube between the lower and upper torches. Since the top flare of the well-known van dermissen burner is surrounded by an enperferpical region that is colored white, yellow, blue and red, depending on the type of material the tube is made from, this area of color will mask characteristic blue n, or green, which may be present. in the core of the upper torch. Therefore, the upper flare cannot be used to detect low concentrations of sulfur and phosphorus. The advantage of the van der Smissen burner is that the excess H2 from the lower torch is burned in the second torch. In addition, since the second torch is always in excess of O2, the second torch will not be extinguished by large emissions of solvent. The first torch is from
    5 times is extinguished by large emissions of solvent, but such a quenching of the first torch is not a problem, because whenever the solvent quenches the first torch, the flame from the second torch automatically lights the first fa; -: ate 2.
    The disadvantage of the Van der Smissssna burner is that. that it is necessary to use a relatively cumbersome water cooling system. Optical observation of the area between two torches must be made not only through the wall of the tube between the two torches, but also through the wall of the water jacket and through
    0 water, which leads to a decrease in sensitivity due to the effects of reflection, refraction and absorption.
    Another disadvantage of the van der Smissen method is that the ze: 1 and 5 bast and the coloration bands due to phosphorus and sulfur, respectively, are in different spatial locations within the luminescence region. Therefore, a change in the mode of selective detection of phosphorus to the mode of selective obium: 1y ke1111 sulfur requires the spatial interaction of the optical axis of the spectrophotometer device observed (for example, a light filter and a photoelectric
    55 lnimntel). In addition, the exact spatial locations of the green and blue bands within the luminescence region strongly depend on the magnitude of the scaling of the incoming gas flows. Pzmenenne
    60 of these CKopocTeii streams may require an additional unbiased optical axis of observation to maintain the optical sensitivity of the iroba.
    With regard to the nitrogenous concentration of the nitrogen compounds by photometric detection using a torch, all known methods are limited by low sensitivity, poor linearity and serious interference from other chemical compounds. In all known analytical methods, the main molecular striped icneKTOp of nitrogen compounds, namely CN, CN, XO, and NH2, was used. In analgesic plumes, it is sometimes seen that "the afterglow of nitrogen occurs as a result of the emission of a continuous spectrum from the reaction N0 + O-XOz + Lg. However, this radiation had previously not used I: I in any analytical method for determining the presence and amount of nitrogen compounds. It is note that the radiation of a wide, even continuous spectrum, as a rule, is less intense and is subject to greater spectral intensity than the pronounced bands of molecular emission of the above-mentioned bands. Radiation from the HNO-HNO-fhr reaction occurs in the spectral range of 650-760 nanometers and is obtained in a hydrogen-rich oxygen-hydrogen plume. However, in this reaction, the main source of interfering radiation is S02.
    The known indicator has a linear sensitivity for nitrogen oxides from 0.15 to 60 hours per million parts. In order to work effectively with this type of fur: For the main class of organic nitrogen compounds, organic nitrogen must be oxidized in a NO or NOo plume. which is difficult to provide in a hydrogen-rich torch.
    The closest in technical essence to; There is a flame sectrotrometer containing a photomultiplier equipped with an integrated system with a housing in which a two-torch burner is installed in the form of two coaxial tubes with pitapn supply channels, and the tip of the inner tube is located below the tip of the outer tube 3.
    The purpose of the invention is to provide precision analysis. A photometric indicator is created in which complex chemical compounds, a complex compound, in the outflow of the gas chromatographic column or contaminants in the atmosphere, are first burned in a hydrogen-rich flame to restore the preconditioning material to the combustion products in a hydrogen-rich flame, in order to bring them into the combustion gases in a hydrogen-rich torch to restore the combustion materials to the combustion products in a hydrogen-rich torch in order to bring them into the combustion gases in a hydrogen-rich torch to restore the combustion materials to the combustion products in the hydrogen-rich torch in order to bring them into the combustion gases in a hydrogen-rich torch in a flame, in order to restore them to the combustion products in the hydrogen-rich flame, to reduce the combustion materials to the combustion materials in the atmosphere, they come before the combustion products in an atmosphere rich in torch, in a hydrogen-rich torch simple chemical structures. The products of combustion and the excess of hydrogen from this first torch are then burned in the second torch, which is separated from the first torch. The second torch provides the torch environment with the radical of a chemical compound with the aim of producing characteristic optical radiation in the second torch, which can be detected by ordinary
    by spectrophotometric conversion. The decomposition of complex chemical compounds in the nerve plume is designed to minimize disturbances in the temperature gradients of the second torch compounds, which could have been possible if complex molecules had entered the second torch.
    The object of the invention is to create a flare photometric indicator which is capable of reliably showing n measures of the sulfur-containing and phosphorus-containing parts of the samples in the samples, and an alimeter for indicating and measuring hydrogen sulfide in the air.
    In addition, it is necessary to create a method of reliable indication and measurement of the presence in the substances of samples containing nitrogen of the e-ions. The nitrogen containing chemical compounds are burned in an oxygen-containing first flare in order to burn nitrous oxide along with other products. Then, nitrogen oxide is passed to the second oxygen-rich torch, in which nitrogen oxide reacts with atomic oxygen to form nitrogen dioxide. The nitrogen dioxide release energy is released in the form of a characteristic light from the first torch. This light can be surrounded by an ectrophotometric means. The method provides for the use of peaKi; i-ii XO + O by an equilibrium reaction obtained by known methods, thus making it possible to detect xsl luminescent molecular recombination of XO and O with the goal of the formation of HO. In the engineering technique, this helper-luminescent recombination was not possible to get enough accuracy for the purpose of repetition of the radiation from other reactions from other reactions. J. Enhance: fakta.ta. This one provides maximum maximally; XO molecules in the fuel for the second ij / key, thereby guaranteeing the diffusion of the first space with a high content of atoms O. in which the XO + O reaction can proceed.
    The aim of the invention is to create a two-torch burner, converted from materials with high specific strength and low impurity content, so that the components of the hot burner contribute to the second torch only:.: Ifiij mallow flame coloring.
    The goal is achieved due to the fact that in a flame spectrophotometer containing a photo-satellite, a connection was established with an optical system with a housing in which a two-torch torch in the form of two coaxial tubes with channels was installed.
    power supply, the inner tube tip is located below the outer tube tip, the burner tube is made of a material with high thermal conductivity, and there is a cylindrical cavity in the case, in which the outer tube of the burner is formed with a gap, forming an annular passage with the cavity walls bottom with at least one cadre for supplying the gas mixture.
    The second torch of the burner is not masked by the imperative region of optical noise, because the excitation of gaseous substances removed from the structural elements of the burner is excluded.
    On fpg. Figure 1 shows a two-flare photometric detection burner, a transverse section; in fig. 2 - the same, together with a spectrophotometric means for observing the upper plume.
    The photometric detection two-flare burner contains the inner and outer elements of the I-II tube tips made from stainless steel, such as stainless steel 316, which has extremely high thermal conductivity compared to fused silica or glass irex. The thermal conductivity of stainless steel 316 in the range of temperatures from 0 to is 0.037, and at a temperature of 650 ° -0.050. The thermal conductivity of molten quartz at room temperature is 0.0033. The thermal conductivity of most types of glass at room temperature is from 0.0016 to 0.0029, with an increase in the value of specific thermal conductivity by 20-25% at a temperature of 200 ° C. Ceramics whose thermal conductivity is close to that of stainless steel can also be used for terminus.
    The internal element of the tip of the tube / is usually a centralized structure with a central opening 3, into which the tip is intended for analyzing a sample, which may be an outflow from the chromatograph of a column. The upper part of the tip of the tube 2 has a tubular shape. Between the outer wall of the storage element of the tube 1 and the inner wall of the element of the tip of the tube 2, an annular gap of 0.254 ml is formed. This annular gap defines the passage for gas flow. The gas flow inlet into the annular passage 4 is provided with one or more pipelines 5,
    A mixture of oxygen-containing gas and gas intended for analysis (nanrnmer, effluent from chromatographic or ambient air sample, which must be analyzed for H2 content) is passed through the central hole 3 of the inner tube tip element /, while hydrogen gas is passed through the pipeline (or pipelines) 5 into the annular passage 4. As a result, the combustion gas mixture PZ central hole 3 is mixed with combustible gas leaving passage 4, h It is necessary to form a hydrogen-rich gas mixture in the area immediately above the upper end of the inner element of the tip of pipe I. In the course of operation, the first flame 6 near the upper part of the element of the tube tip / is ignited by the flame method, which is generated by conventional flame ignition means (e.g. heated spiral), supplied to the upper part of the outer element of the tip of the tube 2. Products cropaiHHH and non-corrosive gases from the first torch 6 go up through the tubular element at the accumulator tube 2 and out of it at a sufficiently distant distance from the upper part of the element of the tube tip. The products of combustion and excess hydrogen from the first flame 6 rise along the element of the tip of the tube 2 to the area where additional oxygen or air is provided, and the second flame 7 is ignited. Usually, in the widest area, the diameter of the element of the tip of the tube 2 is 11.176 ml. To improve the gas mixing, the upper part of the element of the tip of the tube 2 is made conical, reducing the outer 3 of the narrowest part to 4.572 ml. For packers with Bypusta1; with ozone dimensions, the upper part of the element of the tip of the tube 2 protrudes 17,526 mg above the upper part of the element of the tip of the tube /. to other metal parts of the burner in order to dissipate the heat produced by the torch 6 p 7. Consequently, the mini-radiator etsc thermal excitation of gaseous products, beats Tubes I and 2 of the tips. In the case 8 there is a cylindrical cavity in which tube 2 is installed with a gap, forming an annular passage with the cavity walls, which provides a path for oxygen-containing gas, clean air or other gas mixture to pass it through channel 9 and the annular passage before it mixes with the gas Mi coming out of the tip of tube 2
    AND
    in the area located directly above its outer end. This comparatively long path of the notok allows the steady flow of air to be set before mixing it with the gas tubes coming out of the tip of the tube 2, which creates a stabilizing effect on the top flare 7. For the elements of the tips of the sizes given above, the corresponding inner diameter of the cavity of the Cornus 8 is 12.7 ml.
    In the process of operation, the upper torch 7 is ignited by nerves. Then iroskok flame from the upper torch 7 causes ignition of the lower torch 6. If, due to bursts of solvent, the torch sometimes goes out during operation, then the flame from the upper torch 7 automatically causes a new ignition of the lower torch 6.
    The upper torch has a central core, which includes hydrogen and products burned from the torch 6, and the outer shell of an O2 or air. The relative magnitudes of the flow rates of Og or air but channels 5 and 9 n On the pipeline 5, they determine whether flame 7 is predominantly hydrogen-rich or rich in a flare beam source. Favorable photometric detection of compounds containing only sulfur or only phosphorus requires hydrogen-rich surrounding space of torch 7, which can be done by using the following NOTOCOB speeds supported: air but channel 3-80 lgd in 1 min, air but channel 9-170 ml in 1 min, hydrogen but the pipeline 5-140 lgl in 1 min.
    For these gas streams through the burner, the total amount of keporod supplied completely is about 70% of the total amount of hydrogen supplied. Dimensions of poor flows should not be considered restrictive when applied to the invention of the present invention. All sizes can either be increased or reduced to such a rate, while the flow rates of gases will produce steady flames 6 and 7, where torch 7 is rich in hydrogen.
    In the case of hydrogen-rich gas streams containing sulfur and phosphorus, the chemical compounds emit characteristic blue and green colors in the well-defined region of the torch 7 core. These are but the colors. . This is due to the fact that this area of the torch is poorer in oxygen. In the outer flare of the plume, where oxygen is most appreciated, the intensity of sulfur and phosphorus is reduced and the intensity of sulfur is reduced. Both showing sulfur and 12
    The phosphorus-related radiation is dissipated in the same spatial region of the flame 7, which makes it possible to use the same optical axis of observation for any mode of spectral detection. Moreover, in order to remove the tubular size of the tip of the tubing of the Cornus, the spatial area of the upper flare 7, used to detect sulfur n / nli phosphorus, is relatively insensitive to the nominal velocity of the carrier gas carrying the sample substance through the channel o into the lower torch 6, at least in the range of 10 lo 100 ml in 1 min.
    The core area of the upper torch 7 of the burner is not masked by the outer shell of the dye produced by radiation from gaseous substances removed from the hot tips of the torches.
    The radiation from the torch 7 is transmitted through the optical window 10 at the root of the lens 8 to the corresponding lenses // for transmission to a light filter for spectral analysis / 2 selections. The light frequency passing through the filter 12 falls onto a photomultiplier -13, which is connected to a suitable electronic circuit designed to detect the presence of a continuous measurement of the intensity of the interesting chemical compounds in the sample substance. Sometimes it is advisable to replace the filter 12 with a monochromator device.
    In some cases, such as when a cell is found to contain nitrogen-containing chemical compounds, it is required that the upper flare 7 be rich in oxygen. For the burner with the above-specified dimensions of the tip of the tube, the cavity of the torch body 7 can be made oxygen-rich by holding the following speeds and currents: air through channel 3-80 .cl in 1 min, air through channel 9-300 .yl in 1 M-UH, hydrogen through pipelines ;; do 5-70 ml in 1 min.
    For such gas flows through the burner, the total amount of hydrogen iodo and more oxygen is more than enough to consume all the hydrogen supplied. And in this case, ired; 1 sizes; i speed ioroi OB to support () k; 1 w; 1 torch should not be considered restrictive. All dimensions are increased. Л11чн1-; ата or у.1Фие1ат to such walls, so that the receiving speeds of the gas flow rates give stable flares 6 and 7, where the top ::: is; 1 7 is rich in oxygen :.
     hemylummedneptic) CO-r-O - OsOii + hr was observed in flares, in which the combustion product is NO, as in very hot hydrogen (air) flares, where X9 is separated from the air.
    Therefore, due to interfering radiation from other reactions, this reaction is not used for analytical purposes when it detects the presence of, And the amount of chemical compounds containing nitrogen. A quantitative measurement of the nitrogen-containing chemical compounds in the sample is ensured by observing this chemiluminescent reaction in the upper flare 7, where the radiation from other reactions is suppressed.
    Nitrogen-containing compounds of the substance are first burned in the oxygen-containing bottom flare 6 in order to create, along with other combustion products, nitrogen nitrogen. Then XO reacts with oxygen atoms in the upper torch 7 in such a way as to create chemiluminescent formation of XO.
    Due to the non-movement of XO molecules in the area between the two torches, the XO molecules diffuse throughout the entire volume of the oxygen-rich top torch 7, thereby enhancing the possibility of observing the area of the torch in which the reaction occurs.
    The radiation characteristic of the hempluminescent reaction and XO-HO can be observed spectrophotometrically. For optimal detection, it is necessary to use a red-amplifying photomultiplier 13 in combination with filter 12, which transmits light with selected will lengths of more than 500 power meters.
    权利要求:
    Claims (2)
    [1]
    1. Patsit USA X 3489498, cl. 431126. publish 1970.
    [2]
    2. US patent L 3213747, cl. 431-126, iubile. 1968.
    Z. US Patent L 3695813, cl. 431-126, published. 03.10.72 (prototype).
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    同族专利:
    公开号 | 公开日
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    FR2382007A1|1978-09-22|
    DE2806043A1|1978-08-31|
    US4097239A|1978-06-27|
    DE2806043C2|1985-08-08|
    FR2382007B1|1981-10-30|
    CA1093341A|1981-01-13|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/772,710|US4097239A|1977-02-28|1977-02-28|Two-flame burner for flame photometric detection|
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