CN103063596A - Method for detecting tar content in low-tar coke oven gas - Google Patents
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- 239000000571 coke Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 38
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000008096 xylene Substances 0.000 claims abstract description 70
- 238000002835 absorbance Methods 0.000 claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 239000012088 reference solution Substances 0.000 claims description 22
- 238000005070 sampling Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 239000011269 tar Substances 0.000 description 106
- 239000007789 gas Substances 0.000 description 52
- 238000011084 recovery Methods 0.000 description 8
- 238000004737 colorimetric analysis Methods 0.000 description 6
- 230000000007 visual effect Effects 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000011286 gas tar Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
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Abstract
本发明公开了一种检测低焦油(焦油含量在10mg/m3以下)的焦炉煤气中焦油含量的方法，该方法包括以下步骤：(a)获得焦油的二甲苯溶液的焦油浓度与焦油的二甲苯溶液的吸光度之间的线性关系；(b)用二甲苯吸收焦炉煤气中的焦油，得到吸收了焦油的二甲苯；(c)测量吸收了焦油的二甲苯的吸光度，并使用所述线性关系，由吸收了焦油的二甲苯的吸光度获得吸收了焦油的二甲苯的焦油浓度；(d)由吸收了焦油的二甲苯的焦油浓度获得焦炉煤气中的焦油含量。本发明的检测方法可以检测出焦炉煤气中低的焦油含量，具有简单、快速、准确、再现性好等优点。
The invention discloses a method for detecting tar content in coke oven gas with low tar (tar content below 10 mg/m 3 ), the method comprises the following steps: (a) obtaining the tar concentration and the tar content of the xylene solution of tar The linear relationship between the absorbance of xylene solution; (b) absorb the tar in the coke oven gas with xylene, obtain the xylene that has absorbed tar; (c) measure the absorbance of the xylene that has absorbed tar, and use described Linear relationship, the tar concentration of tar-absorbed xylene is obtained from the absorbance of tar-absorbed xylene; (d) The tar content in coke oven gas is obtained from the tar concentration of tar-absorbed xylene. The detection method of the invention can detect low tar content in the coke oven gas, and has the advantages of simplicity, speed, accuracy, good reproducibility and the like.
Description
技术领域technical field
本发明涉及一种焦炉煤气中焦油含量的检测方法，尤其涉及一种低焦油含量(小于10mg/m3)的焦炉煤气中焦油含量的检测方法。The invention relates to a method for detecting tar content in coke oven gas, in particular to a method for detecting tar content in coke oven gas with low tar content (less than 10 mg/m 3 ).
背景技术Background technique
焦炉煤气中焦油含量的检测是衡量焦炉煤气净化后煤气质量的重要参数，也是保障焦炉煤气作为能源供应的重要指标。在冶金领域，焦炉煤气中的焦油雾要进行较彻底的清除，否则将会对焦炉煤气净化带来严重的影响，焦油雾会影响脱硫塔的脱硫效果，因此煤气中焦油含量的分析是焦炉煤气杂质含量检测的最重要检测项目之一。The detection of tar content in coke oven gas is an important parameter to measure the quality of coke oven gas after purification, and also an important indicator to ensure coke oven gas as an energy supply. In the field of metallurgy, the tar mist in the coke oven gas should be removed thoroughly, otherwise it will have a serious impact on the purification of the coke oven gas. The tar mist will affect the desulfurization effect of the desulfurization tower, so the analysis of the tar content in the gas is One of the most important testing items for testing the impurity content of coke oven gas.
现有技术的测定焦炉煤气中焦油含量的一种方法为国标法，即采用GB/T12208-2008《人工煤气组分与杂质含量测定方法》所介绍的方法，通过已知质量的滤膜，以滤膜的质量增加量和取样体积，计算出焦油和灰尘的含量，该方法取样量大，分析时间长，分析结果误差大，而且焦油和灰尘含量不能分开测量。A method for measuring tar content in coke oven gas in the prior art is the national standard method, that is, using the method introduced in GB/T12208-2008 "Artificial Gas Components and Impurity Content Determination Method", through a filter membrane of known quality, The content of tar and dust is calculated based on the mass increase of the filter membrane and the sampling volume. This method has a large sampling volume, a long analysis time, and a large error in the analysis results, and the tar and dust contents cannot be measured separately.
现有技术的测定焦炉煤气中焦油含量的另一种方法为目视比色法。在目视比色法中，采用二甲苯吸收煤气中的焦油，焦油溶解在二甲苯中使二甲苯变色，再与标准系列的二甲苯标准比色液进行比较，得出煤气中焦油含量。焦炉煤气经过固定床干法精脱硫工艺和TSA净化工序后焦炉煤气中的焦油含量基本上低于10mg/m3。对于焦油含量大于10mg/m3的焦炉煤气的焦油含量的测定，目视比色法的测定结果较好，但是对于焦油含量在10mg/m3以下的焦炉煤气的焦油含量的测定，目视比色法的测定结果的误差较大，检测灵敏度低。Another prior art method for determining the tar content in coke oven gas is visual colorimetry. In the visual colorimetric method, xylene is used to absorb the tar in the gas, and the tar is dissolved in the xylene to change the color of the xylene, and then compared with the standard series of xylene standard colorimetric solutions to obtain the tar content in the gas. The tar content in the coke oven gas is basically lower than 10 mg/m 3 after the coke oven gas passes through the fixed bed dry fine desulfurization process and the TSA purification process. For the determination of the tar content of coke oven gas with a tar content greater than 10 mg/m 3 , the visual colorimetric method has better results, but for the determination of the tar content of coke oven gas with a tar content of less than 10 mg/m 3 , the target The error of the measurement result of visual colorimetry is large, and the detection sensitivity is low.
发明内容Contents of the invention
本发明的目的在于解决现有技术的不足，而提供一种适用于低焦油焦炉煤气中焦油含量的检测方法。The purpose of the present invention is to solve the deficiencies of the prior art, and provide a method suitable for detecting tar content in low-tar coke oven gas.
为了实现上述目的，本发明提供一种检测低焦油焦炉煤气中的焦油含量的方法，所述低焦油焦炉煤气中的焦油含量在10mg/m3以下，包括以下步骤：(a)获得焦油的二甲苯溶液的焦油浓度与焦油的二甲苯溶液的吸光度之间的线性关系；(b)用二甲苯吸收焦炉煤气中的焦油，得到吸收了焦油的二甲苯；(c)测量吸收了焦油的二甲苯的吸光度，并使用所述线性关系，由吸收了焦油的二甲苯的吸光度获得吸收了焦油的二甲苯的焦油浓度；(d)由吸收了焦油的二甲苯的焦油浓度获得焦炉煤气中的焦油含量。In order to achieve the above object, the present invention provides a method for detecting tar content in low-tar coke oven gas, wherein the tar content in the low-tar coke oven gas is below 10mg/m , comprising the following steps: (a) obtaining tar The linear relationship between the tar concentration of the xylene solution and the absorbance of the tar xylene solution; (b) absorb the tar in the coke oven gas with xylene to obtain the xylene that has absorbed the tar; (c) measure the absorbed tar and using the linear relationship, obtain the tar concentration of the tar-absorbed xylene from the absorbance of the tar-absorbed xylene; (d) obtain the coke oven gas from the tar concentration of the tar-absorbed xylene tar content in.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，所述步骤(a)可以包括：用二甲苯溶解焦油，制得基准溶液；取不同体积的基准溶液于容量瓶中，用二甲苯定容，得到不同焦油浓度的标样；取一个或多个标样于石英比色皿中，以纯二甲苯为参比溶液，在紫外分光光度计上，波长250～350nm之间检测标样的吸光度，所得吸光度最大的波长作为工作波长；另取标样于石英比色皿中，以纯二甲苯为参比溶液，在紫外分光光度计上的所述工作波长处测定标样的吸光度，并以焦油浓度为横坐标，测定得到的吸光度为纵坐标，绘制标准曲线，并求出回归方程。According to an embodiment of the method for detecting the tar content in low-tar coke oven gas of the present invention, described step (a) can comprise: dissolve tar with xylene, make reference solution; Get the reference solution of different volumes in volumetric flask , constant volume with xylene to obtain standard samples with different tar concentrations; take one or more standard samples in a quartz cuvette, use pure xylene as a reference solution, and use a UV spectrophotometer with a wavelength between 250 and 350nm Detect the absorbance of the standard sample, and the wavelength with the maximum absorbance is used as the working wavelength; another standard sample is taken in a quartz cuvette, and pure xylene is used as a reference solution, and the wavelength of the standard sample is measured at the working wavelength on the ultraviolet spectrophotometer. Absorbance, and with the tar concentration as the abscissa, the measured absorbance as the ordinate, draw a standard curve, and find the regression equation.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，所述工作波长为300nm。According to an embodiment of the method for detecting tar content in low-tar coke oven gas of the present invention, the working wavelength is 300 nm.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，在所述制备基准溶液的步骤中，可以用滤纸进行过滤以去除基准溶液中的渣子，并用加热至40～50℃的二甲苯多次冲洗烧杯和滤纸。According to an embodiment of the method for detecting the tar content in low-tar coke oven gas of the present invention, in the step of preparing the reference solution, filter paper can be used to filter to remove the slag in the reference solution, and heated to 40-50 ° C Rinse the beaker and filter paper several times with xylene.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，在所述步骤(b)中可以控制焦炉煤气的取样量和二甲苯的体积以保证焦油浓度在8～25mg/L之间。According to an embodiment of the method for detecting the tar content in low-tar coke oven gas of the present invention, in described step (b), can control the sampling amount of coke oven gas and the volume of xylene to guarantee tar concentration at 8～25mg/ Between L.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，所述步骤(c)可以包括将吸收了焦油的二甲苯放入石英比色皿中，以纯二甲苯为参比溶液，在紫外分光光度计上的所述工作波长处测定吸光度，并代入所述回归方程中得到焦油浓度。According to one embodiment of the method for detecting the tar content in low-tar coke oven gas of the present invention, said step (c) may include putting the xylene that has absorbed tar into a quartz cuvette, and using pure xylene as a reference solution , measure the absorbance at the working wavelength on the ultraviolet spectrophotometer, and substitute it into the regression equation to obtain the tar concentration.
根据本发明检测低焦油焦炉煤气中的焦油含量的方法的一个实施例，所述步骤(d)可以包括将吸收了焦油的二甲苯的焦油浓度代入公式Z焦油＝C×V1/V0中获得焦炉煤气中的焦油含量，其中，V0＝273×P×V/[760×(273+t)]，式中，Z焦油为标准状态下的焦油含量，mg/Nm3；C为将吸光度代入回归方程计算得到的焦油浓度，mg/L；V1为二甲苯的体积；V0为换算至标准状态下的焦炉煤气取样体积，L；V为取样时焦炉煤气的流量，L；t为取样时焦炉煤气的平均温度，℃；P为取样时的平均大气压力，mmHg。According to one embodiment of the method for detecting tar content in low-tar coke oven gas of the present invention, said step (d) may include substituting the tar concentration of xylene that has absorbed tar into the formula Ztar =C×V 1 /V 0 The tar content in the coke oven gas obtained in the above, wherein, V 0 =273×P×V/[760×(273+t)], where Z tar is the tar content in the standard state, mg/Nm 3 ; C is the tar concentration calculated by substituting the absorbance into the regression equation, mg/L; V 1 is the volume of xylene; V 0 is the sample volume of coke oven gas converted to the standard state, L; V is the flow rate of coke oven gas when sampling , L; t is the average temperature of coke oven gas at the time of sampling, °C; P is the average atmospheric pressure at the time of sampling, mmHg.
与现有技术相比，本发明的有益效果包括适用于焦油含量在10mg/m3以下时的焦炉煤气检测，具有简单、快速、准确、再现性好等优点。Compared with the prior art, the beneficial effects of the present invention include that it is suitable for coke oven gas detection when the tar content is below 10 mg/m 3 , and has the advantages of simplicity, speed, accuracy and good reproducibility.
附图说明Description of drawings
图1是本发明示例性实施例的焦炉煤气中焦油含量的检测方法得到的标准曲线。Fig. 1 is a standard curve obtained by a method for detecting tar content in coke oven gas according to an exemplary embodiment of the present invention.
具体实施方式Detailed ways
在下文中，将结合示例性实施例详细说明本发明的低焦油焦炉煤气中焦油含量的检测方法。Hereinafter, the method for detecting tar content in low-tar coke oven gas of the present invention will be described in detail with reference to exemplary embodiments.
根据本发明的检测低焦油含量(焦油含量在10mg/m3以下)的焦炉煤气中焦油含量的方法，包括以下步骤，(a)获得焦油的二甲苯溶液的焦油浓度与焦油的二甲苯溶液的吸光度之间的线性关系；(b)用二甲苯吸收焦炉煤气中的焦油，得到吸收了焦油的二甲苯；(c)测量吸收了焦油的二甲苯的吸光度，并使用所述线性关系，由吸收了焦油的二甲苯的吸光度获得吸收了焦油的二甲苯的焦油浓度；(d)由吸收了焦油的二甲苯的焦油浓度获得焦炉煤气中的焦油含量。According to the method for tar content in the coke oven gas of detection low tar content (tar content below 10mg/m ) of the present invention, comprise the following steps, (a) obtain the tar concentration of the xylene solution of tar and the xylene solution of tar (b) absorbing tar in coke oven gas with xylene to obtain tar-absorbed xylene; (c) measuring absorbance of tar-absorbed xylene and using said linear relationship, The tar concentration of the tar-absorbed xylene was obtained from the absorbance of the tar-absorbed xylene; (d) the tar content in the coke oven gas was obtained from the tar concentration of the tar-absorbed xylene.
在本发明的一个示例性实施例中，本发明的低焦油焦炉煤气中焦油含量的检测方法可具体通过如下步骤来实现。In an exemplary embodiment of the present invention, the method for detecting tar content in low-tar coke oven gas of the present invention can be specifically implemented through the following steps.
(1)称取0.1g焦油于30mL烧杯中，加入少量二甲苯溶解，用滤纸将溶液中的渣子过滤掉，并用加热至40～50℃的二甲苯多次冲洗烧杯和滤纸，以保证焦油中的渣子都被过滤在滤纸上，待滤纸干燥后称量渣子的质量，得到焦油的纯度。其中，将二甲苯加热至40～50℃是因为焦油的主要成份是多环芳烃，40℃～50℃焦油在二甲苯的可溶解性最佳，且可有效去除焦油中的杂质。(1) Weigh 0.1g of tar into a 30mL beaker, add a small amount of xylene to dissolve it, filter out the residue in the solution with filter paper, and rinse the beaker and filter paper with xylene heated to 40-50°C several times to ensure The slag is filtered on the filter paper, and the quality of the slag is weighed after the filter paper is dried to obtain the purity of the tar. Wherein, heating xylene to 40-50° C. is because the main component of tar is polycyclic aromatic hydrocarbons, and the solubility of tar at 40° C. to 50° C. in xylene is the best, and impurities in tar can be effectively removed.
(2)将过滤后的溶解溶液移入100mL容量瓶中，并用二甲苯多次冲洗烧杯后定容至标线，计算出容量瓶内溶液浓度为0.085mg/mL，并将该溶液作为基准溶液。(2) Transfer the filtered dissolved solution into a 100mL volumetric flask, rinse the beaker with xylene several times, and then set the volume to the marked line. Calculate the solution concentration in the volumetric flask to be 0.085mg/mL, and use this solution as the reference solution.
(3)分别取0.0、0.5、1.0、2.0、4.0、8.0mL所述基准溶液于50mL容量瓶中，用二甲苯定容，得到不同焦油浓度的标样，如表1所示，其中，基准溶液取样体积为0.0mL，焦油浓度为0.0000mg/L的标样是作为参比溶液的纯二甲苯。(3) Take 0.0, 0.5, 1.0, 2.0, 4.0, 8.0mL of the reference solution in a 50mL volumetric flask, dilute to volume with xylene to obtain standard samples of different tar concentrations, as shown in Table 1, wherein the reference The sample volume of the solution is 0.0 mL, and the standard sample with a tar concentration of 0.0000 mg/L is pure xylene as a reference solution.
表1制得的不同焦油浓度的标样The standard sample of different tar concentration that table 1 makes
(4)取一个或多个标样于1cm石英比色皿中，以纯二甲苯为参比溶液，在波长250～350nm之间检测吸光度，找到吸光度最大对应的波长作为工作波长，这里，选择吸光度最大时对应的波长作为工作波长的原因是由于最大吸收波长处摩尔吸光系数最大、测定灵敏度最高、检测误差最小，所以将吸光度最大的波长选为工作波长。(4) Take one or more standard samples in a 1cm quartz cuvette, use pure xylene as a reference solution, detect the absorbance at a wavelength of 250-350nm, and find the wavelength corresponding to the maximum absorbance as the working wavelength. Here, select the absorbance The reason why the wavelength corresponding to the maximum is used as the working wavelength is that the molar absorptivity at the maximum absorption wavelength is the largest, the measurement sensitivity is the highest, and the detection error is the smallest, so the wavelength with the largest absorbance is selected as the working wavelength.
以焦油浓度为8.5mg/mL(I)和17mg/mL(II)的标样为例，在波长250～350nm之间检测得到的吸光度如表2所示。Taking the standard samples with a tar concentration of 8.5 mg/mL (I) and 17 mg/mL (II) as examples, the absorbance measured at a wavelength of 250-350 nm is shown in Table 2.
表2标样I和II检测得到的吸光度Table 2 Absorbance obtained by standard sample I and II detection
由表2可以看出，在波长300nm处吸光度最大，因此工作波长为300nm。It can be seen from Table 2 that the absorbance is maximum at the wavelength of 300nm, so the working wavelength is 300nm.
(5)取所述标样于1cm石英比色皿中，以纯二甲苯为参比溶液，在紫外分光光度计上的工作波长300nm处测定各个标样的吸光度，结果如表3所示：(5) get described standard sample in 1cm quartz cuvette, take pure xylene as reference solution, measure the absorbance of each standard sample at the operating wavelength 300nm place on the ultraviolet spectrophotometer, the results are as shown in table 3:
表3不同焦油浓度的标样检测得到的吸光度The absorbance obtained by the standard sample detection of table 3 different tar concentrations
以焦油浓度为横坐标，测定得到的吸光度为纵坐标，绘制标准曲线，如图1所示，并求出回归方程为：Take the tar concentration as the abscissa, measure the absorbance obtained as the ordinate, draw a standard curve, as shown in Figure 1, and obtain the regression equation as:
C＝0.0026+0.0711A，r＝0.99962 (1)C＝0.0026+0.0711A, r＝0.99962 (1)
上式中，A为吸光度；C为焦油浓度，mg/L；r为相关系数。In the above formula, A is the absorbance; C is the tar concentration, mg/L; r is the correlation coefficient.
(6)测定回收率，具体包括以下步骤：(6) Determination of recovery, specifically comprises the following steps:
①取50mL上述0.085mg/mL的基准溶液倒入100mL容量瓶中，用二甲苯多次冲洗后定容，计算出容量瓶内溶液浓度42.016mg/L，并将该溶液作为测回收率的标准溶液备用。①Pour 50mL of the above-mentioned 0.085mg/mL reference solution into a 100mL volumetric flask, rinse with xylene several times and then constant volume, calculate the concentration of the solution in the volumetric flask as 42.016mg/L, and use this solution as the standard for measuring the recovery rate The solution is ready for use.
②分别取5.0、6.0、7.0、8.0、9.0、10.0、11.0、12.0mL制得的标准溶液于50mL容量瓶中，得到不同焦油浓度的标样，如表4所示，用二甲苯定容，盖紧塞子摇匀。其中，标准溶液浓度与加标样量之积为实际值。② Take 5.0, 6.0, 7.0, 8.0, 9.0, 10.0, 11.0, 12.0mL of the prepared standard solution in a 50mL volumetric flask to obtain standard samples with different tar concentrations, as shown in Table 4, dilute to volume with xylene, Cap tightly and shake well. Among them, the product of the concentration of the standard solution and the volume of the standard sample is the actual value.
③以纯二甲苯为参比溶液，在紫外分光光度计上的工作波长300nm处测步骤②所得标样的吸光度，并根据所得的吸光度在从标准曲线中查出其所对应的焦油浓度，或者将所得的吸光度代入回归方程式(1)中得到焦油浓度，焦油浓度与标样的体积50mL之积为回收值。回收率等于回收值与实际值之比，结果如表4所示。③ Take pure xylene as the reference solution, measure the absorbance of the standard sample obtained in
表4测定回收率的结果Table 4 measures the result of recovery rate
从表4可以看出，测定回收率平均为98.1％，即采用紫外分光光度计测量焦油浓度的测量准确度高。As can be seen from Table 4, the measured recovery rate is 98.1% on average, that is, the measurement accuracy of the tar concentration measured by the ultraviolet spectrophotometer is high.
(7)将吸收了焦炉煤气的二甲苯溶液放入1cm石英比色皿中，以纯二甲苯为参比溶液，在紫外分光光度计上的工作波长300nm处测定吸光度，所得的吸光度代入回归方程式(1)中，得到焦油浓度，再用以下公式求出焦炉煤气中的焦油含量：(7) Put the xylene solution that has absorbed coke oven gas into a 1cm quartz cuvette, take pure xylene as a reference solution, and measure the absorbance at the operating wavelength 300nm on the UV spectrophotometer, and the resulting absorbance is substituted into the regression equation (1), obtain the tar concentration, then use the following formula to find the tar content in the coke oven gas:
Z焦油＝C×V1/V0 (2)Z tar = C × V 1 /V 0 (2)
上式中，Z焦油为标准状态下的焦油含量，mg/Nm3；C为将吸光度代入回归方程计算得到的焦油浓度，mg/L；V1为二甲苯的体积；V0为换算至标准状态下(760mmHg，0℃)的焦炉煤气取样体积，L；In the above formula, Z tar is the tar content in the standard state, mg/Nm 3 ; C is the tar concentration calculated by substituting the absorbance into the regression equation, mg/L; V 1 is the volume of xylene; V 0 is converted to the standard Sampling volume of coke oven gas under state (760mmHg, 0°C), L;
V0＝273×P×V/(760×(273+t)) (3)V 0 =273×P×V/(760×(273+t)) (3)
V为取样时的煤气流量，L；t为取样时煤气的平均温度，℃；P为取样时的平均大气压力，mmHg。V is the gas flow rate at the time of sampling, L; t is the average temperature of the gas at the time of sampling, °C; P is the average atmospheric pressure at the time of sampling, mmHg.
由于紫外分光光度计也会有一定的测量误差，而从标准曲线上可以看出，吸光度在0.04～0.9内测量值准确性较高，因此，控制所述焦炉煤气的取样量和二甲苯的体积，保证焦油浓度在8～25mg/L之间，可以提高计算的准确度。Because the ultraviolet spectrophotometer also has certain measurement errors, and as can be seen from the standard curve, the accuracy of the measured value of the absorbance is higher in 0.04～0.9, therefore, control the sampling amount of the coke oven gas and xylene The volume, to ensure the tar concentration between 8 ~ 25mg/L, can improve the accuracy of the calculation.
以下，将目视比色法和本发明的方法进行对比以进一步说明本发明的检测方法，两种测定焦油含量的方法的对比结果如表5所示，可以看出采用目视比色法本身误差相对较大，对于焦油含量大于10mg/m3时检测效果比较好，而当焦油含量低于10mg/m3时，该方法的检测灵敏度低，基本检测不出来，因此，采用标准色阶比色法会造成分析结果误差较大，难以准确掌握净化后焦炉煤气焦油真实含量，而采用本发明的检测方法可以解决上述问题。Below, the visual colorimetry and the method of the present invention are compared to further illustrate the detection method of the present invention, the comparison result of two kinds of methods of measuring tar content is as shown in table 5, it can be seen that adopting visual colorimetry itself The error is relatively large, and the detection effect is better when the tar content is greater than 10 mg/m 3 , but when the tar content is lower than 10 mg/m 3 , the detection sensitivity of this method is low and basically cannot be detected. Therefore, the standard color scale ratio is used The color method will cause large errors in the analysis results, and it is difficult to accurately grasp the real content of the purified coke oven gas tar, but the detection method of the present invention can solve the above problems.
表5两种测定焦油含量的方法的对比结果The comparison result of two kinds of methods of measuring tar content in table 5
综上所述，采用本发明的方法可以对经过煤气净化系统净化后焦炉煤气中焦油含量的进行准确测定，特别适用于焦油含量在10mg/m3以下时的焦炉煤气检测，测定回收率平均为98.1％，具有简单、快速、准确、再现性好等特点。本方法不但可用于焦炉煤气，对其他煤气的焦油含量也可以适用。In summary, the method of the present invention can be used to accurately measure the tar content in the coke oven gas purified by the gas purification system, and is particularly suitable for coke oven gas detection when the tar content is below 10mg/ m3 , and the recovery rate is determined The average is 98.1%. It has the characteristics of simplicity, speed, accuracy and good reproducibility. This method is not only applicable to coke oven gas, but also applicable to the tar content of other gases.
尽管上面已经通过结合示例性实施例描述了本发明，但是本领域技术人员应该清楚，在不脱离权利要求所限定的精神和范围的情况下，可对本发明的示例性实施例进行各种修改和改变。Although the present invention has been described above in conjunction with the exemplary embodiments, it should be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope defined in the claims. Change.
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