CN103018192B - 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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- CN103018192B CN103018192B CN201310014681.2A CN201310014681A CN103018192B CN 103018192 B CN103018192 B CN 103018192B CN 201310014681 A CN201310014681 A CN 201310014681A CN 103018192 B CN103018192 B CN 103018192B
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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 drilling fluid.
Background technology
The quantitative test of polyethers non-ionic surfactant has instrumental method and chemical method.Can directly adopt 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 has picrate method (0. 1～1mg/L), oscilloscopic polarography (0. 1～2. 6mg/L) and tetraiodo cadmium potassium association extraction atomic absorption method (0.07～3 mg/L) etc.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 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.
A kind of method that therefore, need to provide in situ quantitation to analyze polyether glycol in 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 quantitative test drilling fluid.
The absorbance of the first on-site measurement of the present invention drilling fluid medium-Si, Mo to be measured acid, the corresponding content of searching polyether glycol in drilling fluid to be measured from the absorbance of drilling fluid medium-Si, Mo acid and the linear relationship typical curve of the content of polyether glycol 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, after finishing, reaction adds again excess silicon molybdic acid, the centrifugal precipitation of removing of system again reaction being formed, get supernatant, measure the absorbance of excess silicon molybdic acid with ultraviolet spectrophotometer.
It is acid that the present invention regulates drilling fluid to arrive by hydrochloric acid, disturb by the foreign ion that adds excessive barium chloride to reduce in drilling fluid, then add silicomolybdic acid, make silicomolybdic acid and barium chloride, polyether glycol three form precipitation, in the supernatant obtaining, contain excess silicon molybdic acid and a small amount of barium chloride.Finally measure the absorbance of excess silicon molybdic acid with ultraviolet spectrophotometer, then can obtain the content of polyether glycol in drilling fluid by 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 features such as sensitivity, accuracy are high, favorable reproducibility, and the present invention locates out peak value in 210nm left and right.In the absorbance of drilling fluid medium-Si, Mo of the present invention acid and drilling fluid, the linear relationship typical curve of the content of polyether glycol can be made in advance, only need carry out absorbance test to drilling fluid to be measured at the scene, therefore, can adopt small portable spectrophotometer, realize the object of the content of polyether glycol in collection in worksite, fast-field evaluation drilling fluid.
The making step of linear relationship typical curve of the present invention is:
1) take quantitatively not containing the drilling fluid of polyether glycol, add quantitative polyether glycol titer, mix.Drilling fluid is diluted at least five parts of standard polyether polyatomic alcohol drilling fluids that preparation contains different polyether glycol concentration respectively with deionization;
2) get respectively standard polyether polyatomic alcohol drilling fluid described in 3.5mL step 1) and be placed in respectively each centrifuge tube, then in each centrifuge tube, drip aqueous hydrochloric acid solution respectively, the pH value that makes mixed system in each centrifuge tube is 2～3; Then in each centrifuge tube, add respectively the barium chloride that 1mL quality percentage composition is 30% to react, after finishing, question response in each centrifuge tube, add respectively the silicomolybdic acid aqueous solution that 100.00 μ L quality percentage compositions are 5% to react again, after question response finishes, centrifugal 5min under the condition that is 9000r/min respectively at rotating speed by each centrifuge tube, obtains respectively supernatant;
3) after each supernatant is diluted respectively, measure respectively the absorbance of each supernatant medium-Si, Mo acid with ultraviolet spectrophotometer, and absorbance peak value when obtaining wavelength and being 210nm;
4) the absorbance peak value while described wavelength corresponding to described every part of standard polyether polyatomic alcohol drilling fluid being 210nm is made in standard polyether polyatomic alcohol drilling fluid, to contain polyether glycol concentration in horizontal ordinate, graph of a relation taking absorbance peak value as ordinate, again each mark line in graph of a relation is connected in line, obtain the content linear relationship typical curve of absorbance and polyether glycol.
Above-mentioned steps 1) in polyether glycol be the block polymer of polyoxyethylene and polyoxypropylene.
The present invention compared with prior art has following good effect:
1, cost of the present invention is low, and analytic process is simple and quick.More than 90%, can be weighed the feasibility of this analytical approach by recovery of standard addition.Be less than 5% by relative standard deviation, can illustrate that the reappearance of this analytical approach is better.The present invention can solve polyether glycol content in the drilling fluid of complicated component and be not easy to the technical matters of measuring thus.
2, the present invention can implement on-the site analysis.Adopt 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 initial drilling fluid, improve the efficiency that drilling fluid composition is adjusted, reduce unnecessary material consumption, thereby reduce cost.
3, the complex that silicomolybdic acid, barium chloride and polyether glycol form within a certain period of time absorbance is stable.
4, sodium silicate, sodium molybdate, barium chloride, hydrochloric acid are the standing reagent in laboratory, cheap and easy to get, and its related solution is easy to preparation, is not subject to the interference of human factor.These reagent solutions have higher stability, can preserve for a long time.
Brief description of the 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 250mL volumetric flask, accurately take respectively 7 parts of 15g drilling fluids, add the polyether glycol standard sample of different quality, make polyether glycol massfraction be respectively 0,0.3495%, 0.7006 %, 1.025%, 1.431 %, 1.873 %, 2.294%, use 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.In 7 centrifuge tubes, add respectively the barium chloride that 1mL quality percentage composition is 30% to react, after finishing, question response in 7 centrifuge tubes, add respectively the silicomolybdic acid aqueous solution that 100.00 μ l quality percentage compositions are 5% to react again, after question response finishes, centrifugal 5min under the condition that is 9000r/min respectively at rotating speed by 7 centrifuge tubes, obtains respectively 7 portions of supernatants.
3,7 portions of supernatants are diluted respectively to 50 times, measure respectively the absorbance of 7 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and absorbance peak value when obtaining 7 groups of wavelength and being 210nm.As shown in Figure 1.
In Fig. 1, the spectrogram curve of a-g represents that the concentration of polyether glycol in 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.
4, the absorbance peak value while 7 parts of described 7 groups of wavelength corresponding to standard polyether polyatomic alcohol drilling fluid being 210nm is made in standard polyether polyatomic alcohol drilling fluid, to contain polyether glycol concentration in horizontal ordinate, graph of a relation taking absorbance peak value as ordinate, again 7 mark lines in 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 on-the-spot drilling fluid sample:
1, take the drilling fluid of 15.0027g, with 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, in 5 centrifuge tubes, add respectively the barium chloride that 1mL quality percentage composition is 30% to react, after finishing, question response in 5 centrifuge tubes, add respectively the silicomolybdic acid aqueous solution that 100.00 μ L quality percentage compositions are 5% to react again, after question response finishes, centrifugal 5min under the condition that is 9000r/min respectively at rotating speed by 5 centrifuge tubes, obtains respectively 5 portions of supernatants.
5,5 portions of supernatants are diluted respectively to 50 times, measure respectively the absorbance of 5 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and absorbance peak value when obtaining 5 groups of wavelength and being 210nm, in table 1:
| Sequence number | 1 | 2 | 3 | 4 | 5 |
| 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 each upper table absorbance peak value being made with Fig. 2 contrasts, and obtains the content of polyether glycol in 5 on-the-spot drilling fluid samples, as shown in the table:
| Sequence number | 1 | 2 | 3 | 4 | 5 |
| Content (%) | 0.99 | 1.01 | 1.02 | 0.99 | 1.03 |
Average, draw: the content of the polyether glycol in on-the-spot drilling fluid sample is 1.01%.
Claims (2)
1. the method for polyether glycol content in an 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 drilling fluid to be measured from the absorbance of drilling fluid medium-Si, Mo acid and the linear relationship typical curve of the content of polyether glycol drilling fluid; The method of the absorbance of described on-site measurement drilling fluid medium-Si, Mo to be measured acid is:
Take the drilling fluid of 15.0027g, with deionized water dilution, constant volume is to 250mL; Again with 5 times of deionized water dilutions;
Get 5 centrifuge tubes, add respectively the water-reducible drilling fluid of the above-mentioned deionization of 3.5mL;
In 5 centrifuge tubes, add respectively an aqueous hydrochloric acid solution, the pH value that makes mixed system in 5 centrifuge tubes is 2;
In 5 centrifuge tubes, add respectively the barium chloride that 1mL quality percentage composition is 30% to react, after finishing, question response in 5 centrifuge tubes, add respectively the silicomolybdic acid aqueous solution that 100.00 μ L quality percentage compositions are 5% to react again, after question response finishes, centrifugal 5min under the condition that is 9000r/min respectively at rotating speed by 5 centrifuge tubes, obtains respectively 5 portions of supernatants;
5 portions of supernatants are diluted respectively to 50 times, measure respectively the absorbance of 5 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and absorbance peak value when obtaining 5 groups of wavelength and being 210nm; Each absorbance peak value is contrasted with linear relationship typical curve, obtain the content of polyether glycol in 5 on-the-spot drilling fluid samples, average;
The method for making of described linear relationship typical curve is:
1) take respectively 7 parts of 15g drilling fluids, add the polyether glycol standard sample of different quality, make polyether glycol massfraction be respectively 0,0.3495%, 0.7006 %, 1.025%, 1.431 %, 1.873 %, 2.294%, with deionized water constant volume to 250mL, then with 5 times of deionized water dilutions;
2) get 7 centrifuge tubes, 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, the pH value that makes mixed system in 7 centrifuge tubes is 2; In 7 centrifuge tubes, add respectively the barium chloride that 1mL quality percentage composition is 30% to react, after finishing, question response in 7 centrifuge tubes, add respectively the silicomolybdic acid aqueous solution that 100.00 μ L quality percentage compositions are 5% to react again, after question response finishes, centrifugal 5min under the condition that is 9000r/min respectively at rotating speed by 7 centrifuge tubes, obtains respectively 7 portions of supernatants;
3) 7 portions of supernatants are diluted respectively to 50 times, measure respectively the absorbance of 7 parts of supernatant medium-Si, Mos acid with ultraviolet spectrophotometer, and absorbance peak value when obtaining 7 groups of wavelength and being 210nm;
4) the absorbance peak value while 7 parts of described 7 groups of wavelength corresponding to standard polyether polyatomic alcohol drilling fluid being 210nm is made in standard polyether polyatomic alcohol drilling fluid, to contain polyether glycol concentration in horizontal ordinate, graph of a relation taking absorbance peak value as ordinate, again 7 mark lines in graph of a relation are connected in line, obtain the content linear relationship typical curve of absorbance and polyether glycol.
2. the method for polyether glycol content in on-site measurement drilling fluid according to claim 1, is characterized in that: in step 1), polyether glycol is the block polymer of polyoxyethylene and polyoxypropylene.
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| 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 |
| 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 |
| 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 |
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 |
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| 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 |
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