阅读说明：本技术 一种新型测定复垦土地样品中石油类的方法 (Novel method for determining petroleum in reclaimed land sample ) 是由 赵江华 李忠煜 韩延兵 张明祖 李艳广 于 2019-08-28 设计创作，主要内容包括：本发明属于土壤样品中石油类测定技术领域,公开了一种加速溶剂萃取-荧光分光光度法测定复垦土地样品中石油类的方法,采用加速溶剂萃取仪对土壤样品的石油类组分进行提取、浓缩及净化处理,获得待测定提取液；对获得待测定提取液进行固定激发波长激发和测定荧光强度,然后利用标准工作曲线进行土壤样品中石油类浓度计算。本发明采用加速溶剂萃取仪进行土壤样品的提取,有效的对样品中的石油类组分进行了提取,溶剂用量小,提取效率高,仪器自动化；本发明荧光分光光度法的测定既准确又简便,在保证测试结果准确可靠的同时也大大提高了分析测试的效率。(The invention belongs to the technical field of determination of petroleum in soil samples, and discloses a method for determining petroleum in reclaimed land samples by using an accelerated solvent extraction-fluorescence spectrophotometry, wherein an accelerated solvent extractor is used for extracting, concentrating and purifying petroleum components in the soil samples to obtain an extracting solution to be determined; and (3) exciting the obtained extracting solution to be measured by using a fixed excitation wavelength and measuring the fluorescence intensity, and then calculating the concentration of petroleum in the soil sample by using a standard working curve. The soil sample is extracted by adopting the accelerated solvent extractor, so that the petroleum components in the sample are effectively extracted, the solvent consumption is small, the extraction efficiency is high, and the apparatus is automatic; the fluorescence spectrophotometry method of the invention is accurate, simple and convenient, and greatly improves the efficiency of analysis and test while ensuring the accuracy and reliability of the test result.)

1. A method for determining petroleum species in a reclaimed land sample, said method for determining petroleum species in a reclaimed land sample using accelerated solvent extraction-fluorescence spectrophotometry, comprising:

firstly, extracting and concentrating petroleum components of a soil sample by adopting an accelerated solvent extractor;

secondly, purifying to obtain an extracting solution to be measured;

thirdly, measuring the concentration of the sample by a fluorescence spectrophotometer; and (3) exciting the obtained extracting solution to be measured by using a fixed excitation wavelength and measuring the fluorescence intensity, and then calculating the concentration of petroleum in the soil sample by using a standard working curve.

2. The method of assaying for petroleum species in a reclaimed land sample of claim 1, wherein the first step specifically comprises:

the method adopts an accelerated solvent extractor to carry out extraction operation, and the collection and extraction of the extraction solution comprises the following steps: weighing 10.0g of sample in a 34ml extraction tank, adding treated diatomite to fill the space of an extraction tank, taking n-hexane as an extraction solvent, extracting at 80 ℃, under the extraction pressure of 1200psi, performing static extraction for 5min, leaching to 60% of the tank volume, purging with nitrogen for 60s, performing extraction cycle times of 2 times, and collecting the extraction solution.

3. The method for assaying petroleum species in a reclaimed land sample according to claim 1, wherein the second step of the purification treatment of the extraction solution specifically comprises the steps of:

(1) blowing the extract to 10ml above nitrogen, and manually purifying with commercial solid phase extraction column;

(2) activating the small column by using a normal hexane solvent with the volume of 1-2 column tubes;

(3) adding all the extractive solution into the small column, and collecting effluent;

(4) eluting the small column with n-hexane, draining the liquid, collecting effluent, and mixing the effluent of the two times;

(5) the mixture was concentrated to 10ml by nitrogen-blowing.

4. The method for assaying petroleum species in a reclaimed land sample according to claim 1, wherein the third step of spectrofluorometric assay of the sample concentration specifically comprises: and (3) measuring by adopting a concentration mode, wherein the widths of excitation and emission slits are both 5mm, the excitation wavelength is 310nm, the emission wavelength is 360nm, the integration time is 1s, the background value is automatically subtracted, the quartz cuvette is 10mm, and the existing working curve is called for calculation to obtain the concentration of the sample.

5. The method for assaying for petroleum species in a reclaimed land sample of claim 4, wherein the petroleum species content in the sample is obtained by the calculation of the following equation:

in the formula: rho represents the mass concentration of petroleum in the soil, and the unit is mg/kg; c represents the measured concentration in mg/L; v represents the volume of the extract in ml; m represents the weight in g.

6. An accelerated solvent extraction-fluorescence spectrophotometry assay for petroleum-like systems in reclaimed land samples for carrying out the method of any one of claims 1 to 5, wherein the accelerated solvent extraction-fluorescence spectrophotometry assay for petroleum-like systems in reclaimed land samples comprises:

the accelerated solvent extraction instrument is used for extracting, concentrating and purifying petroleum components of the soil sample to obtain an extracting solution to be measured;

and the fluorescence spectrophotometer is used for exciting the obtained extracting solution to be measured by using a fixed excitation wavelength and measuring the fluorescence intensity, and then calculating the concentration of petroleum in the soil sample by using a standard working curve.

7. The accelerated solvent extraction-fluorescence spectrophotometry assay for petroleum-like systems in reclaimed land samples of claim 6, wherein the accelerated solvent extractor comprises:

a liquid suction pump for sucking the solvent;

a nitrogen purge instrument for performing nitrogen purge on the absorbed solvent;

injecting a solvent purged by nitrogen into the extraction tank;

and a collecting bottle for collecting the extracted extracting solution.

8. The accelerated solvent extraction-fluorescence spectrophotometry assay of petroleum-like systems in reclaimed land samples of claim 7 wherein the nitrogen purge meter controls the rate of nitrogen purge via a purge valve.

9. The accelerated solvent extraction-fluorescence spectrophotometry assay of petroleum-like components of a reclaimed land sample of claim 7 wherein the extraction cell controls the flow rate of extraction fluid to the collection vial via a static valve.