Gravimetric method and device for measurement of moist content in moisture-containing organic material, particularly, in timber

FIELD: measurement engineering.

SUBSTANCE: moisture is extracted from moisture-containing organic material, for example, from timber. Device is used which has pressure-tight chambers for removing moisture, carriages for loading organic materials, moisture collectors and heat lines. Weight of removed moisture in relation to weight of organic material is calculated.

EFFECT: reduced time of procedure; increased precision of testing.

3 cl, 5 dwg

 

The invention relates to the field of determining moisture content and other thermally extractable substances in organic materials having a capillary structure, including wood, including materials of synthetic origin.

Known indirect methods for determining moisture content in organic materials and sell their devices, based on the measurement of parameters that depend on moisture content, such as conductivity, dielectric constant, etc. the Main disadvantage of indirect methods is the need for prior calibration of measurement systems for each type of the investigated material with the use of direct methods for the determination of moisture content.

To well-known direct methods of determining moisture content are dried at 105°C to constant mass, distillation of water with a nonpolar organic solvent, subtitling reagent Fisher (G. Kononov. Chemistry of wood and its main components. - M.: 1999, 247 S.), of which the most common and close in fact present invention is a standard drying method according to GOST 11014-81 (with subsequent amendments). This method is repeated determination of the mass of the test sample moisture-containing material in the drying process when the temperature is 105° C. drying and weighing continue up until the mass of the sampled material will not cease to decrease. The resulting drying substance is considered "absolutely dry", and relative (WREL) or absolute (Wabs) the moisture content of the source material in a percentage determined by the formula

where mW- initial sample mass of material, mabsthe mass of absolutely dry substance obtained from the initial sample of the material in the drying at a temperature of about 105°to stabilize the mass.

The most significant disadvantage of the standard method is that the drying process at a temperature of 105°and multiple weighing samples long. In addition, the accuracy of determination of moisture by this method is low because not all the moisture held in the capillaries of the plant tissue may be removed at the same temperature drying. The selection of bound moisture from organic material in significant (up to 300...400° (C) increase in temperature would lead to the fact that due to thermal degradation of the organic matter together with the moisture of the solids are removed and degradation products.

The aim of the invention is the reduction product is littelest procedures for determining the amount of moisture, contained in the organic materials of plant origin and increase the accuracy of determining the amount of moisture due to its more complete separation from the studied material, as well as the opportunity to determine the content of different types of moisture released from the studied organic material at different temperatures.

This technical result is achieved by the gravimetric method of determining the moisture content of the sample crushed investigated moisture-containing organic material is quickly heated to a temperature in the range of 105...375°over time, which in the studied organic matter do not have time to occur chemical processes, in particular with the participation of the contained moisture by thermal contact with the heated surface of the heat transfer material in concurrent mechanical pressure is applied to this surface. Selection and determination of the mass of moisture removed from the organic material at different temperatures, are produced at different temperatures a few cameras. After determining the mass of extracted moisture carry out an analysis of its composition.

The invention is disclosed using figure 1-5. Figure 1 presents the design of a device for separating moisture from one sample alternately in multiple to the measures and figure 2 shows a device for separating moisture out of several sub-samples of organic material. Figure 3-5 shows the three main phases of operation of the device separating moisture for one camera Department moisture on the proposed method of determination of its content in organic material.

The device in figure 1 includes several sealed chambers remove moisture 1 (the number of chambers of moisture removal is determined by the amount of moisture content, the content of which you want to analyze), boot the carriage 2 with the cavity 3 bounded from below by a thin partition 4 from a material with high thermal conductivity, and a few (by number of cameras remove moisture) drives moisture 6. Each of the drives moisture 6 communicates with one of the chambers of moisture removal 1. To ensure the collection of moisture released from the organic matter, the drive moisture 6 is equipped with a refrigerator and / or regenerated adsorption element 7, and may simultaneously be working chamber chromatograph. To prevent condensation from moisture in the walls of the chamber to remove moisture and drive their heated by the heater 14. The device operates as follows.

A portion of the crushed moisture-containing organic material 5, the mass of which is taken for mWplaced in the cavity 3 of the carriage 2. Then slide the RAM is moved into the first chamber to remove moisture where at the temperature T1 is separated moisture, temperature extraction from organic matter less than or equal to T1. After that, the carriage with the sample is transferred into the second chamber to remove moisture and released from the sample moisture is completely distilled to drive moisture 6 which is connected with the first chamber to remove moisture and weighed; the weight of this moisture is taken for mWW1. In the second chamber to remove moisture sample is heated at a temperature T2 and produce the removal of her moisture, temperature selection, which lies in the range T1...T2, after which the carriage with the sample moved into the next chamber to remove moisture and released from the sample in the second chamber to remove moisture in distilled communicated with her drive moisture and weighed; the weight of this moisture is taken for mWW2. The above procedure for removal, distillation and weighing moisture repeat for all cameras remove moisture at temperatures, respectively, T1, T2, ...Tn, where T1<T2<T3<...<Tn, T1=105°S, Tn≤375°C. the Mass of moisture removed from the organic material at temperatures T1, T2, ...Tn-1, take mWW1, mWW1, ...mWWnrespectively. Then, determine the mass of a sample after separation from it of moisture in the last chamber at the temperature Tn, take it for mabs. Then calculate the relative (WkREL) or absolute (Wkabs) the content is of different types of moisture, released at the temperature Tk by formulas

where k is a positive integer and 1<k<n.

After weighing the moisture released from the organic material at different temperatures, produce chromatographic or other analysis of its composition.

The device in figure 2, is designed to separate the moisture on the "parallel" scheme, includes several sealed chambers remove moisture 1 (the number of chambers of moisture removal is determined by the amount of moisture content, the content of which you want to analyze), and the same number of boot carriage 2 with the cavity 3 bounded from below by a thin partition 4 from a material with high thermal conductivity. The device operates as follows.

First, cook N (the number of types of moisture content which you want to analyze) hanging investigated chopped moisture-containing organic material 5. A lot of the first, second, etc. hanging accept, respectively, for mW1, ..., mW2, ..., mWk, ..., mWn. Each of the hanging moisture-containing organic material is placed in one of the boot of the carriage 2, then each carriage 2 is introduced into one of the chambers of moisture removal 1. Each of the cells 1 to produce the removal of moisture from placed in her sample of organic the ski material at a temperature T1, T2, ..., Tk ... or Tk, where T1<T2<T3<...<Tn, T1=105°S, Tn≤375°C. After removal of moisture from hanging the moisture-containing organic material they weighed again and take their mass, respectively: mWM1, mWM2...mWMk, ...mWMn. Then calculate the relative (WkREL) or absolute (Wkabscontents of various types of moisture released during the temperature Tk by the formulas:

where k is a positive integer and 1<k<N.

Figure 3-5 shows three stages in the process of removing moisture in one of the cells 1. The camera 1 includes the heat pipes 8 and 11 with the heating elements 9. In the lower part of the upper heat pipe 8, provided with the clamping device 13, there is a system of channels 10 for withdrawal of moisture vapour from the lower surface of the heat pipe 12 into the internal cavity of the chamber 1. Figure 3 shows the initial phase of the process of moisture removal, when the cavity 3 of the boot of the carriage 2 is located outside of the gap between the heat pipes 8 and 11, the temperature of which is maintained constant and equal to the desired value Tk in the range of 105...375°C. Hitch 5 investigated slurry of organic material placed in the cavity 3 of the boot of the carriage 2. Then boot the carriage side quickly move in a horizontal plane so that it Polo is th 3 was between the working surfaces 12 of the heat pipes 8 and 11, as shown in figure 4. After that, the upper heat 8 quickly lowered and with the help of the clamping device 13 is tightly compress the portion 5 of the investigated material with thermally conductive wall 4 between heated to the required temperature of the working surface 12 of the heat pipes 8 and 11. This phase of the process is presented in figure 5. Due to constant thermal contact and mechanical pressure applied perpendicular to the surface of contact of organic material with heat pipes, carry out rapid heating of the entire volume of the sample to the desired temperature Tk for the time (less than 1), which does not occur chemical modification of the investigated organic material. The process of moisture removal is in the nature of "microexplosion", in which there is intensive emission of moisture from the amount of organic material, as it formed a closed microregions, filled with pairs of boiling moisture, which due to internal pressure to break through the layer of organic material on its surface. The channel system 10 of the upper heat pipe provides a more rapid withdrawal of moisture from the heating zone into the internal cavity of the camera 1.

After the moisture to be removed at a given temperature Tk, will be displayed in the internal cavity of the chamber 1, the upper heat pipe 9 is raised, and loading the loading carriage 2 with organic material is displayed and the camera 1.

To ensure rapid and uniform heating of the sample moisture-containing organic material to its initial (before you put it in the camera 1) mass mWkmust meet at least one of the two following conditions:

where M is the total mass of the heat pipes 8 and 11,

cmand cm- specific heat capacity, respectively, of the investigated material and the material of the heat,

mWWkis the mass of the moisture released from the sample mWkin the chamber to remove moisture at a temperature Tk,

λk- heat of vaporization at temperature Tk,

k - coefficient of heat losses in heat transfer through

the heat pipes 8 and 11 and the partition wall 4 to the hinge of the studied material;

2) the power of the heaters 9 should be sufficient to maintain a constant heat flux, providing heating of the sample to the desired temperature Tk in the range of 105...375°for the time at which the removal of moisture is in the nature of "microexplosion" (<1). For the limiting case, when the relative humidity of organic material is close to 100%, and at temperatures below the critical temperature of water (about 374°C)the flow of heat to the sample of organic material must be above 4 kW per one gram sample of organic material.

1. Gravimetricheskie determine the moisture content in the moisture-containing organic material, in particular in the wood, by calculating the ratio of the mass of moisture to the mass of organic material, characterized in that the extraction of moisture from the at least one hinge moisture-containing organic material and determining the moisture content of exercise due to thermal contact with the heat pipes in several chambers of moisture removal at different temperatures in the range 105...375°by heating the moisture-containing organic material over time, which does not occur chemical modification of organic material, simultaneously exerting mechanical pressure on the moisture-containing organic material perpendicular to the surface of its contact with the heat pipes, the heat flow energy to the sample moisture-containing organic material should be not less than 4 kW per gram of sample released moisture is collected in separate enclosures are equipped with refrigerators or sorption elements weighed.

2. Device for collecting moisture in the determination of the moisture content in the moisture-containing organic material, in particular wood, containing a sealed chamber to remove moisture and installed in her carriage to load the moisture-containing organic material, characterized in that it further comprises a sealed chamber removed what I moisture, which number corresponds to the number of drives moisture, equipped with a fridge or sorption element, each airtight chamber to remove moisture contains two located one above the other of the heat from a material with high thermal conductivity, equipped with heaters with a total capacity of not less than 4 kW per gram of the investigated aqueous organic material, and lower the heat fixed, and the upper heat pipe having in the lower part of the channel system for the pair, can move reciprocating in a vertical plane and provided with a clamping device for maintaining constant thermal contact between the heat pipes with moisture-containing organic material, and the number of carriages moving in the horizontal plane corresponds to the number of cameras remove moisture.



 

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