CN110542733A - Method for determination of petroleum sulfonate concentration in oil well production fluid by liquid chromatography analysis - Google Patents
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- 239000003208 petroleum Substances 0.000 title claims abstract description 45
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 44
- 239000003129 oil well Substances 0.000 title claims abstract description 28
- 239000012530 fluid Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000004458 analytical method Methods 0.000 title claims abstract description 6
- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000005349 anion exchange Methods 0.000 claims abstract description 6
- 238000010829 isocratic elution Methods 0.000 claims abstract description 5
- 238000010812 external standard method Methods 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000012267 brine Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000000825 ultraviolet detection Methods 0.000 description 2
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
本发明公开了利用液相色谱分析测定油井采出液中石油磺酸盐浓度的方法，其色谱条件为：色谱柱为10 cm SAX强阴离子交换柱；流动相为甲醇与0.02 mol/LNH4Ac水溶液混合液，且体积比3/2，流速1.0 mL/min，等度洗脱；采用紫外检测器检测，检测波长225 nm；20µL进样，测定石油磺酸盐的紫外色谱峰面积，外标法定量。在5~500 mg/L内，石油磺酸盐的浓度与色谱峰面积之间的线性关系为：Y=‑93.358+12.126 X，线性相关系数R=0.99965。本发明检测油井采出水中石油磺酸盐，具有简单、准确、快速、灵敏、检出限低、重复性好等特点。The invention discloses a method for measuring the concentration of petroleum sulfonate in oil well production fluid by using liquid chromatography analysis. The chromatographic conditions are as follows: the chromatographic column is a 10 cm SAX strong anion exchange column; the mobile phase is methanol and 0.02 mol/L NH 4 Ac aqueous solution Mixed solution, with a volume ratio of 3/2, a flow rate of 1.0 mL/min, and isocratic elution; detected by a UV detector with a detection wavelength of 225 nm; 20 µL of sample was injected to determine the UV chromatographic peak area of petroleum sulfonate, external standard method Quantitative. In the range of 5-500 mg/L, the linear relationship between the concentration of petroleum sulfonate and the chromatographic peak area is: Y=-93.358+12.126 X, and the linear correlation coefficient R=0.99965. The invention detects the petroleum sulfonate in the water produced by the oil well, and has the characteristics of simplicity, accuracy, speed, sensitivity, low detection limit, good repeatability and the like.
Description
技术领域technical field
本发明涉及一种油井采出液中石油磺酸盐浓度的测定方法，尤其涉及一种采用高效液相色谱法测定油井采出液中石油磺酸盐浓度的方法，属于油田化学分析技术领域。The invention relates to a method for measuring the concentration of petroleum sulfonate in oil well production fluid, in particular to a method for measuring the concentration of petroleum sulfonate in oil well production fluid by using high performance liquid chromatography, and belongs to the technical field of oilfield chemical analysis.
背景技术Background technique
表面活性剂在二元复合驱采油、三元复合驱采油中发挥着十分重要的作用，其作用机理在于有效降低油水界面张力，增强体系乳化性能，进而提高原油采收率。作为一类常用的表面活性剂，石油磺酸盐被广泛的应用于三次采油领域，其结构由烷基芳基疏水基团与磺酸根阴离子基团两部分组成的阴离子表面活性剂。为了开展石油磺酸盐油井采出水中检出量与驱油效率之间的量效关系，石油磺酸盐在油藏环境中的运移规律、吸附损耗等研究，需要对油井采出液中的石油磺酸盐浓度进行准确检测，这就要求建立油井采出液中石油磺酸盐的浓度检测方法。Surfactant plays a very important role in binary compound flooding and ASP flooding. Its mechanism of action is to effectively reduce the interfacial tension of oil and water, enhance the emulsification performance of the system, and improve oil recovery. As a commonly used surfactant, petroleum sulfonate is widely used in the field of tertiary oil recovery. Its structure is an anionic surfactant composed of two parts: alkylaryl hydrophobic group and sulfonate anion group. In order to carry out the study on the amount-effect relationship between the detected amount of petroleum sulfonate in oil well produced water and the oil displacement efficiency, the migration law and adsorption loss of petroleum sulfonate in the reservoir environment, it is necessary to study the To accurately detect the concentration of petroleum sulfonate, this requires the establishment of a detection method for the concentration of petroleum sulfonate in oil well production fluid.
石油磺酸盐的浓度检测方法包括滴定法、比色法等，但是，这些方法操作繁琐、灵敏度低、重现性差，针对油井采出液这一复杂基质环境，抗干扰能力低，难以实现石油磺酸盐的准确检测。此外，针对石油磺酸盐的浓度检测，中国科学院兰州化学物理研究所建立了一套以5 cm SAX强阴离子交换柱为色谱柱，以甲醇/水、甲醇/0.25 mol/L NaH2PO4水溶液分别为流动相，梯度洗脱的高效液相色谱分析检测方法，该方法具有准确、快速、灵敏的特点，但缺点在于流动相中含有大量NaH2PO4无机盐，往往因为无机盐的析出导致色谱流路堵塞，给分析工作带来麻烦，同时，梯度洗脱也不利于普通油田分析测试人员的掌握。因此，十分有必要开发一种更为简单的石油磺酸盐高效液相色谱分析检测方法。The concentration detection methods of petroleum sulfonate include titration method, colorimetry, etc. However, these methods are cumbersome to operate, low in sensitivity, and poor in reproducibility. Accurate detection of sulfonates. In addition, for the concentration detection of petroleum sulfonate, the Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences established a set of 5 cm SAX strong anion exchange columns as chromatographic columns, using methanol/water, methanol/0.25 mol/L NaH 2 PO 4 aqueous solution The mobile phase and the high-performance liquid chromatography detection method of gradient elution, this method has the characteristics of accuracy, rapidity and sensitivity, but the disadvantage is that the mobile phase contains a large amount of NaH 2 PO 4 inorganic salts, which is often caused by the precipitation of inorganic salts. The blockage of the chromatographic flow path brings troubles to the analysis work. At the same time, the gradient elution is not conducive to the grasp of ordinary oilfield analysis and testing personnel. Therefore, it is very necessary to develop a simpler HPLC analysis and detection method for petroleum sulfonate.
发明内容Contents of the invention
本发明的目的是提供一种液相色谱测定油井采出液中石油磺酸盐浓度的方法。The object of the invention is to provide a method for liquid chromatography to measure petroleum sulfonate concentration in oil well production fluid.
本发明液相色谱定量检测油井采出液中石油磺酸盐的方法，包括以下内容：The method for quantitative detection of petroleum sulfonate in oil well production fluid by liquid chromatography of the present invention comprises the following contents:
色谱柱：10 cm SAX强阴离子交换柱；Chromatographic column: 10 cm SAX strong anion exchange column;
流动相：甲醇与0.02 mol/L NH4Ac水溶液混合液，且体积比3/2；流速1.0 mL/min，等梯度洗脱；Mobile phase: mixed solution of methanol and 0.02 mol/L NH 4 Ac aqueous solution, and the volume ratio is 3/2; flow rate 1.0 mL/min, isocratic elution;
紫外检测器：检测波长225 nm；UV detector: detection wavelength 225 nm;
样品的制备：分别用油田注入水配制系列不同浓度的石油磺酸盐标准品溶液（5、10、20、50、100、200、500、1000 mg/L）；Sample preparation: Prepare a series of petroleum sulfonate standard solutions (5, 10, 20, 50, 100, 200, 500, 1000 mg/L) with oilfield injection water;
在上述色谱条件下进样，20 μL进样；测定石油磺酸盐的色谱峰面积，外标法定量石油磺酸盐的浓度。以峰面积积分值为纵坐标，以对照品浓度为横坐标，经线性回归处理得标准曲线（见图1）。Under the above chromatographic conditions, inject 20 μL of sample; measure the chromatographic peak area of petroleum sulfonate, and quantify the concentration of petroleum sulfonate by external standard method. Take the integral value of the peak area as the ordinate, and take the concentration of the reference substance as the abscissa, and obtain the standard curve through linear regression processing (see Figure 1).
结果表明，在20~500 mg/L范围内，石油磺酸盐的浓度与色谱峰面积之间具有良好的线性关系，且具体线性方程为：The results showed that within the range of 20-500 mg/L, there was a good linear relationship between the concentration of petroleum sulfonate and the chromatographic peak area, and the specific linear equation was:
Y = -93.358 + 12.126 X，线性相关系数R = 0.99965Y = -93.358 + 12.126 X, linear correlation R = 0.99965
其中，X——石油磺酸盐的浓度，单位mg/LAmong them, X—concentration of petroleum sulfonate, unit mg/L
Y——色谱峰面积，单位：Intens。Y——chromatographic peak area, unit: Intens.
检出限测定：色谱条件同上，将石油磺酸盐浓度不断稀释，测定其色谱峰响应强度，确定了该方法检出限可以低至2 mg/L。Determination of detection limit: The chromatographic conditions are the same as above, the concentration of petroleum sulfonate is continuously diluted, and the response intensity of the chromatographic peak is measured. It is determined that the detection limit of this method can be as low as 2 mg/L.
重复性测试：色谱条件同上，将50 mg/L的石油磺酸盐分别在第一天、第三天、第五天进样，测定色谱峰面积，考察数据的重复性。经测定，色谱峰面积分别为466.2、484.7、492.3，经计算，相对标准偏差为2.79%，较小，说明数据的重复性很好。Repeatability test: The chromatographic conditions are the same as above, 50 mg/L petroleum sulfonate was injected on the first day, the third day, and the fifth day respectively, and the chromatographic peak area was measured to investigate the repeatability of the data. After measurement, the chromatographic peak areas were 466.2, 484.7, and 492.3 respectively. After calculation, the relative standard deviation was 2.79%, which was small, indicating that the repeatability of the data was very good.
油井采出液加标回收率实验：往丙5A237、丙6A235、7A237三组油井采出液中添加50 ppm石油磺酸盐，20 μL进样，测定峰面积，然后扣除本底峰面积，依据线性关系，计算测定浓度，测定浓度对比50 ppm，获得油井采出液中的加标回收率，见表1：Oil well production fluid spiked recovery experiment: Add 50 ppm petroleum sulfonate to three groups of oil well production fluids of C5A237, C6A235, and 7A237, inject 20 μL of sample, measure the peak area, and then deduct the background peak area, according to Linear relationship, calculate the measured concentration, and compare the measured concentration with 50 ppm to obtain the recovery rate of the standard addition in the oil well production fluid, see Table 1:
由表1可以看出，三组油井采出液中石油磺酸盐的加标回收率均在95.84%至102.26%之间，证实了所提供的高效液相色谱定量检测油井采出液中石油磺酸盐方法的可靠性。It can be seen from Table 1 that the recovery rates of petroleum sulfonate in the production fluid of the three groups of oil wells are all between 95.84% and 102.26%, which confirms the quantitative detection of petroleum sulfonate in the production fluid of the oil well by the provided high performance liquid chromatography. The reliability of the salt method.
综上所述，本发明检测油井采出液中的石油磺酸盐的高效液相色谱方法，具有简单、准确、快速、灵敏、检出限低、重复性好等特点。In summary, the HPLC method for detecting petroleum sulfonate in oil well production fluid of the present invention has the characteristics of simplicity, accuracy, rapidity, sensitivity, low detection limit, and good repeatability.
附图说明Description of drawings
图1为石油磺酸盐的浓度-色谱峰面积之间的线性关系。Fig. 1 is the linear relationship between the concentration of petroleum sulfonate-chromatographic peak area.
图2 为200 mg/L的石油磺酸盐的色谱图。Figure 2 is the chromatogram of 200 mg/L petroleum sulfonate.
具体实施方式Detailed ways
下面通过具体实施例对本发明高效液相色谱分析检测油井采出液中的石油磺酸盐的浓度分析方法作进一步说明。The method for analyzing and detecting the concentration of petroleum sulfonate in oil well production fluid by high performance liquid chromatography of the present invention will be further described below through specific examples.
实施例1Example 1
1、待测样品配制：6AT216油井采出水、6A237油井采出水中石油磺酸盐浓度测定；1. Preparation of samples to be tested: Determination of petroleum sulfonate concentration in 6AT216 oil well produced water and 6A237 oil well produced water;
2、检测2. Detection
色谱条件：10 cm SAX强阴离子交换柱为色谱柱；甲醇与0.02 mol/L NH4Ac水溶液混合液（体积比3/2）为流动相，流速1.0 mL/min，等梯度洗脱；紫外检测器，225 nm检测波长检测； Chromatographic conditions: 10 cm SAX strong anion exchange column as chromatographic column; methanol and 0.02 mol/L NH 4 Ac aqueous solution mixture (volume ratio 3/2) as mobile phase, flow rate 1.0 mL/min, isocratic elution; UV detection detector, 225 nm detection wavelength detection;
在上述色谱条件下，20 μL进样油井采出水，在5.07 min无石油磺酸盐色谱峰，证明2种油井采出水中不含有石油磺酸盐。 Under the above chromatographic conditions, 20 μL of oil well produced water was injected, and there was no petroleum sulfonate chromatographic peak at 5.07 min, which proved that the two kinds of oil well produced water did not contain petroleum sulfonate.
实施例2Example 2
1、样品配制：分别用蒸馏水、油井模拟盐水、6AT216油井采出水、6A237油井采出水配制浓度为50 mg/L的石油磺酸盐溶液；1. Sample preparation: use distilled water, oil well simulated brine, 6AT216 oil well produced water, and 6A237 oil well produced water to prepare petroleum sulfonate solutions with a concentration of 50 mg/L;
2、检测2. Detection
色谱条件：10 cm SAX强阴离子交换柱为色谱柱；甲醇与0.02 mol/L NH4Ac水溶液混合液（体积比3/2）为流动相，流速1.0 mL/min，等梯度洗脱；紫外检测器，225 nm检测波长检测； Chromatographic conditions: 10 cm SAX strong anion exchange column as chromatographic column; methanol and 0.02 mol/L NH 4 Ac aqueous solution mixture (volume ratio 3/2) as mobile phase, flow rate 1.0 mL/min, isocratic elution; UV detection detector, 225 nm detection wavelength detection;
在上述色谱条件下，20 μL进样上述加标溶液，石油磺酸盐均在5.07 min出峰（见图2），测定不同水溶液中石油磺酸盐的色谱峰面积； Under the above-mentioned chromatographic conditions, 20 μL of the above-mentioned spiked solution was injected, and the petroleum sulfonate peaked at 5.07 minutes (see Figure 2). The chromatographic peak areas of petroleum sulfonate in different aqueous solutions were determined;
根据线性关系：Y = -93.358 + 12.126 X，计算出蒸馏水、油井模拟盐水、6AT216油井采出水、6A237油井采出水等不同水溶液中石油磺酸盐的浓度，分别为47.62 mg/L、48.26 mg/L、53.73 mg/L、52.26 mg/L，与50 mg/L相当，证明检测方法的可靠性。 According to the linear relationship: Y = -93.358 + 12.126 X, the concentration of petroleum sulfonate in distilled water, oil well simulated brine, 6AT216 oil well produced water, 6A237 oil well produced water and other aqueous solutions were calculated, which were 47.62 mg/L and 48.26 mg/L respectively , 53.73 mg/L, 52.26 mg/L, equivalent to 50 mg/L, proving the reliability of the detection method.
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| CN112229940A (en) * | 2020-11-27 | 2021-01-15 | 中国科学院兰州化学物理研究所 | Method for the detection of alkyl alcohol polyoxyethylene ether sulfate in crude oil by liquid chromatography |
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Application publication date: 20191206 |