CN103018192A - Method of determining polyether polyol content in drilling fluid in field - Google Patents
Method of determining polyether polyol content in drilling fluid in field Download PDFInfo
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- CN103018192A CN103018192A CN2013100146812A CN201310014681A CN103018192A CN 103018192 A CN103018192 A CN 103018192A CN 2013100146812 A CN2013100146812 A CN 2013100146812A CN 201310014681 A CN201310014681 A CN 201310014681A CN 103018192 A CN103018192 A CN 103018192A
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Abstract
The invention provides a method of determining the polyether polyol content in a drilling fluid in field, belonging to the technical field of chemical analysis of the drilling fluids. The method comprises the following steps of: determining the absorbance of silicomolybdic acid in the drilling fluid in the field firstly, and correspondingly searching the polyether polyol content in the drilling fluid to be detected from a linear relation standard curve of the absorbance of the silicomolybdic acid in the drilling fluid and the polyether polyol content in the drilling fluid. The method has the characteristics of wide application range, high sensitivity and accuracy, good reproducibility and the like. According to the method provided by the invention, a peak value occurs at about 210nm; and the linear relation standard curve of the absorbance of the silicomolybdic acid in the drilling fluid and the polyether polyol content in the drilling fluid can be made in advance, the absorbance of the drilling fluid to be detected only needs to be tested in the field, and therefore, a portable small-sized spectrophotometer can be adopted, thus reaching the purposes of collecting and rapidly determining the polyether polyol content in the drilling fluid in the field.
Description
Technical field
The invention belongs to the chemical analysis technology field of drilling fluid, particularly in situ quantitation is analyzed the method for polyether glycol content in the drilling fluid.
Background technology
The quantitative test of polyethers non-ionic surfactant has instrumental method and chemical method.Can directly adopt the spectrphotometric method for measuring except APES class non-ionic surfactant contains benzene ring structure, generally all adopt chemical determination.The detection method of polyether glycol have the picrate method (0. 1～1mg/L), oscilloscopic polarography (0. 1～2. 6mg/L) and the tetraiodo cadmium potassium extraction atomic absorption method (0.07～3 mg/L) etc. that associates.Although these method accuracy are high, sensing range is little, and complicated operation and disturbing factor are many.Picrate method, cobalt sulphur cyanogen ammonium development process length consuming time, complex steps adopts the toxic reagent environmental pollution larger.Thiocyanation cadmium complexometric extraction atomic absorption method and anodic stripping voltammetry are not easy to make miniature instrument, can not be used for on-site measurement.
The method that therefore, need to provide a kind of in situ quantitation to analyze polyether glycol in the drilling fluid solves the problems referred to above.
Summary of the invention
The object of the present invention is to provide a kind of scene easily and fast, the method for polyether glycol content in the quantitative test drilling fluid.
The absorbance of the present invention elder generation on-site measurement drilling fluid medium-Si, Mo to be measured acid, the corresponding content of searching polyether glycol in the drilling fluid to be measured in the linear relationship typical curve of the content of polyether glycol from the absorbance of drilling fluid medium-Si, Mo acid and drilling fluid; The method of the absorbance of described on-site measurement drilling fluid medium-Si, Mo to be measured acid is: after drilling fluid to be measured is diluted with deionized water, with salt acid for adjusting pH value to 2～3, add excessive barium chloride, reaction adds the excess silicon molybdic acid after finishing again, to react again the centrifugal precipitation of removing of system that forms, get supernatant, measure the absorbance of excess silicon molybdic acid with ultraviolet spectrophotometer.
The present invention regulates drilling fluid by hydrochloric acid and arrives acid, disturb by the foreign ion that adds in the excessive barium chloride minimizing drilling fluid, then add silicomolybdic acid, make silicomolybdic acid and barium chloride, polyether glycol three form precipitation, contain excess silicon molybdic acid and a small amount of barium chloride in the supernatant that obtains.Measure at last the absorbance of excess silicon molybdic acid with ultraviolet spectrophotometer, can obtain again the content of polyether glycol in the drilling fluid by the linear relationship typical curve.
Because polyether glycol just forms lurid precipitation under barium chloride, the simultaneous condition of silicomolybdic acid, otherwise form blueness or dark blue solution, produce blue shift, and the non-linear relation of the content of this absorbance and polyether glycol.So the present invention requires barium chloride excessive.
The method has and has wide range of applications, the characteristics such as sensitivity, accuracy are high, favorable reproducibility, and the present invention locates out peak value about 210nm.The linear relationship typical curve of the content of polyether glycol can be made in advance in the absorbance of drilling fluid medium-Si, Mo of the present invention acid and the drilling fluid, only need at the scene drilling fluid to be measured is carried out the absorbance test, therefore, can adopt the small portable spectrophotometer, realize the purpose of the content of polyether glycol in collection in worksite, the fast-field evaluation drilling fluid.
The making step of linear relationship typical curve of the present invention is:
1) takes by weighing the drilling fluid that does not quantitatively contain polyether glycol, add quantitative polyether glycol titer, mix.Drilling fluid is diluted with deionization, and preparation contains at least five parts of standard polyether polyatomic alcohol drilling fluids of different polyether glycol concentration respectively;
2) get respectively the described standard polyether polyatomic alcohol drilling fluid of 3.5mL step 1) and place respectively each centrifuge tube, then drip aqueous hydrochloric acid solution respectively in each centrifuge tube, the pH value that makes mixed system in each centrifuge tube is 2～3; Then adding respectively 1mL quality percentage composition in each centrifuge tube and be 30% barium chloride reacts, adding respectively 100.00 μ L quality percentage compositions after question response finishes in each centrifuge tube again and be 5% silicomolybdic acid aqueous solution reacts, after question response finishes, be centrifugal 5min under the condition of 9000r/min respectively at rotating speed with each centrifuge tube, obtain respectively supernatant;
3) each supernatant is diluted respectively after, measure respectively the absorbance of each supernatant medium-Si, Mo acid with ultraviolet spectrophotometer, and the absorbance peak value when obtaining wavelength and being 210nm;
Absorbance peak value when 4) described wavelength corresponding to described every part of standard polyether polyatomic alcohol drilling fluid being 210nm is made in and contains polyether glycol concentration in the standard polyether polyatomic alcohol drilling fluid in horizontal ordinate, graph of a relation take the absorbance peak value as ordinate, again each mark line in the graph of a relation is connected in line, obtain the content linear relationship typical curve of absorbance and polyether glycol.
Above-mentioned steps 1) polyether glycol is the block polymer of polyoxyethylene and polyoxypropylene in.
The present invention compared with prior art has following good effect:
1, cost of the present invention is low, the analytic process Simple fast.By recovery of standard addition in the feasibility that can weigh this analytical approach more than 90%.Less than 5%, can illustrate that the reappearance of this analytical approach is better by relative standard deviation.The present invention can solve the technical matters that polyether glycol content is not easy to measure in the drilling fluid of complicated component thus.
2, the present invention can implement on-the site analysis.Adopt the small portable spectrophotometer, implement collection in worksite drilling fluid sample, and the content of polyether glycol in this drilling fluid of analytical calculation.Can judge fast and efficiently the addition of the polyether glycol in the initial drilling fluid, improve the efficient that drilling fluid composition is adjusted, reduce unnecessary material consumption, thereby reduce cost.
3, absorbance is stable within a certain period of time for the complex of silicomolybdic acid, barium chloride and polyether glycol formation.
4, sodium silicate, sodium molybdate, barium chloride, hydrochloric acid are the standing reagent in laboratory, and is cheap and easy to get, and its related solution is easy to preparation, is not subjected to the interference of human factor.These reagent solutions have higher stability, but long preservation.
Description of drawings
Fig. 1 is the curve of spectrum of different polyether glycol concentration.
Fig. 2 is the linear relationship chart of polyether glycol concentration and maximum absorbance.
Embodiment
One, the drafting of linear relationship typical curve:
1, in the 250mL volumetric flask, accurately takes by weighing respectively 7 parts of 15g drilling fluids, add the polyether glycol standard sample of different quality, make the polyether glycol massfraction be respectively 0,0.3495%, 0.7006 %, 1.025%, 1.431 %, 1.873 %, 2.294%, use the deionized water constant volume to 250mL.For subsequent use with 5 times of deionized water dilutions again.
2, get the centrifuge tube of 7 5mL, add respectively the above-mentioned 7 parts of standard polyether polyatomic alcohol drilling fluids of 3.5mL, then add respectively an aqueous hydrochloric acid solution (V
HCl: V
H2O=1:4), the pH value that makes mixed system in 7 centrifuge tubes is 2.Adding respectively 1mL quality percentage composition in 7 centrifuge tubes and be 30% barium chloride reacts, adding respectively 100.00 μ l quality percentage compositions after question response finishes in 7 centrifuge tubes again and be 5% silicomolybdic acid aqueous solution reacts, after question response finishes, be centrifugal 5min under the condition of 9000r/min respectively at rotating speed with 7 centrifuge tubes, obtain respectively 7 portions of supernatants.
3,7 portions of supernatants are diluted respectively 50 times, measure respectively the absorbance of 7 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and the absorbance peak value when obtaining 7 groups of wavelength and being 210nm.As shown in Figure 1.
Among Fig. 1, the concentration that the spectrogram curve of a-g represents polyether glycol in the standard polyether polyatomic alcohol drilling fluid is respectively: 0,0.3495%, 0.7006 %, 1.025 %, 1.431 %, 1.873 %, 2.294%.
As seen from Figure 1, the absorbance peak value of 7 curves appears at respectively 210nm wavelength place.
Absorbance peak value when 4,7 parts of described 7 groups of wavelength corresponding to standard polyether polyatomic alcohol drilling fluid being 210nm is made in and contains polyether glycol concentration in the standard polyether polyatomic alcohol drilling fluid in horizontal ordinate, graph of a relation take the absorbance peak value as ordinate, again 7 mark lines in the graph of a relation are connected in line, obtain the content linear relationship typical curve of absorbance and polyether glycol.As shown in Figure 2.
Two, the mensuration of polyether glycol in the on-the-spot drilling fluid sample:
1, take by weighing the drilling fluid of 15.0027g, with the deionized water dilution, constant volume is to 250mL.Again with 5 times of deionized water dilutions.
2, get the centrifuge tube of 5 5mL, add respectively the water-reducible drilling fluid of the above-mentioned deionization of 3.5mL.
3, in 5 centrifuge tubes, add respectively an aqueous hydrochloric acid solution (V
HCl: V
H2O=1:4), the pH value that makes mixed system in 5 centrifuge tubes is 2.
4, adding respectively 1mL quality percentage composition in 5 centrifuge tubes is that 30% barium chloride reacts, adding respectively 100.00 μ L quality percentage compositions after question response finishes in 5 centrifuge tubes again and be 5% silicomolybdic acid aqueous solution reacts, after question response finishes, be centrifugal 5min under the condition of 9000r/min respectively at rotating speed with 5 centrifuge tubes, obtain respectively 5 portions of supernatants.
5,5 portions of supernatants are diluted respectively 50 times, measure respectively the absorbance of 5 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and the absorbance peak value when obtaining 5 groups of wavelength and being 210nm, see Table 1:
| |
1 | 2 | 3 | 4 | 5 |
| The absorbance peak value | 0.504 | 0.499 | 0.496 | 0.505 | 0.494 |
Table 1 is the absorbance peak value of 5 parts of supernatant medium-Si, Mos acid
6, the linear relationship typical curve contrast that each absorbance peak value of upper table and Fig. 2 is made namely obtains the content of polyether glycol in 5 on-the-spot drilling fluid samples, and is as shown in the table:
| |
1 | 2 | 3 | 4 | 5 |
| Content (%) | 0.99 | 1.01 | 1.02 | 0.99 | 1.03 |
Average, namely draw: the content of the polyether glycol in the on-the-spot drilling fluid sample is 1.01%.
Claims (3)
1. the method for polyether glycol content in the on-site measurement drilling fluid, it is characterized in that: the absorbance of first on-site measurement drilling fluid medium-Si, Mo to be measured acid, the corresponding content of searching polyether glycol in the drilling fluid to be measured in the linear relationship typical curve of the content of polyether glycol from the absorbance of drilling fluid medium-Si, Mo acid and drilling fluid; The method of the absorbance of described on-site measurement drilling fluid medium-Si, Mo to be measured acid is: after drilling fluid to be measured is diluted with deionized water, with salt acid for adjusting pH value to 2～3, add excessive barium chloride, reaction adds the excess silicon molybdic acid after finishing again, to react again the centrifugal precipitation of removing of system that forms, get supernatant, measure the absorbance of excess silicon molybdic acid with ultraviolet spectrophotometer.
2. the method for polyether glycol content in the described on-site measurement drilling fluid according to claim 1, it is characterized in that: the method for making of described linear relationship typical curve is:
1) takes by weighing the drilling fluid that does not quantitatively contain polyether glycol, add quantitative polyether glycol titer, mix; Drilling fluid is diluted with deionization, and preparation contains at least three parts of standard polyether polyatomic alcohol drilling fluids of different polyether glycol concentration respectively;
2) get respectively the described standard polyether polyatomic alcohol drilling fluid of 3.5mL step 1) and place respectively each centrifuge tube, then drip aqueous hydrochloric acid solution respectively in each centrifuge tube, the pH value that makes mixed system in each centrifuge tube is 2～3; Then adding respectively 1mL quality percentage composition in each centrifuge tube and be 30% barium chloride reacts, adding respectively 100.00 μ L quality percentage compositions after question response finishes in each centrifuge tube again and be 5% silicomolybdic acid aqueous solution reacts, after question response finishes, be centrifugal 5min under the condition of 9000r/min respectively at rotating speed with each centrifuge tube, obtain respectively supernatant;
3) each supernatant is diluted respectively after, measure respectively the absorbance of each supernatant medium-Si, Mo acid with ultraviolet spectrophotometer, and the absorbance peak value when obtaining wavelength and being 210nm;
Absorbance peak value when 4) described wavelength corresponding to described every part of standard polyether polyatomic alcohol drilling fluid being 210nm is made in and contains polyether glycol concentration in the standard polyether polyatomic alcohol drilling fluid in horizontal ordinate, graph of a relation take the absorbance peak value as ordinate, again each mark line in the graph of a relation is connected in line, obtain the content linear relationship typical curve of absorbance and polyether glycol.
3. the method for polyether glycol content in the described on-site measurement drilling fluid according to claim 2, it is characterized in that: polyether glycol is the block polymer of polyoxyethylene and polyoxypropylene in the described step 1).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323412A (en) * | 2018-12-13 | 2020-06-23 | 中石化石油工程技术服务有限公司 | On-site monitoring method for content of amino polyether in drilling fluid filtrate |
| CN111380826A (en) * | 2018-12-27 | 2020-07-07 | 中国石油天然气股份有限公司 | Method and device for detecting drilling fluid performance |
| CN112986162A (en) * | 2019-12-16 | 2021-06-18 | 中国石油天然气股份有限公司 | Method and device for judging drilling fluid inhibition |
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| US6676903B2 (en) * | 2001-07-30 | 2004-01-13 | General Electric Company | Apparatus and method for spatially detecting or quantifying chemical species |
| CN102141511A (en) * | 2010-01-28 | 2011-08-03 | 中国石油化工集团公司 | Device and method for measuring molecular weight of polyether or polyether ester |
| CN102313707A (en) * | 2011-08-03 | 2012-01-11 | 中粮生物化学（安徽）股份有限公司 | Method for determining silicon dioxide content in substances containing citric acid |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6676903B2 (en) * | 2001-07-30 | 2004-01-13 | General Electric Company | Apparatus and method for spatially detecting or quantifying chemical species |
| CN102141511A (en) * | 2010-01-28 | 2011-08-03 | 中国石油化工集团公司 | Device and method for measuring molecular weight of polyether or polyether ester |
| CN102313707A (en) * | 2011-08-03 | 2012-01-11 | 中粮生物化学（安徽）股份有限公司 | Method for determining silicon dioxide content in substances containing citric acid |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323412A (en) * | 2018-12-13 | 2020-06-23 | 中石化石油工程技术服务有限公司 | On-site monitoring method for content of amino polyether in drilling fluid filtrate |
| CN111380826A (en) * | 2018-12-27 | 2020-07-07 | 中国石油天然气股份有限公司 | Method and device for detecting drilling fluid performance |
| CN111380826B (en) * | 2018-12-27 | 2022-12-02 | 中国石油天然气股份有限公司 | Method and device for detecting drilling fluid performance |
| CN112986162A (en) * | 2019-12-16 | 2021-06-18 | 中国石油天然气股份有限公司 | Method and device for judging drilling fluid inhibition |
| CN112986162B (en) * | 2019-12-16 | 2023-04-25 | 中国石油天然气股份有限公司 | Method and device for judging drilling fluid inhibition |
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