CN101592644B - Method for detecting barium ions in oil field water - Google Patents
Method for detecting barium ions in oil field water Download PDFInfo
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- CN101592644B CN101592644B CN2009103037702A CN200910303770A CN101592644B CN 101592644 B CN101592644 B CN 101592644B CN 2009103037702 A CN2009103037702 A CN 2009103037702A CN 200910303770 A CN200910303770 A CN 200910303770A CN 101592644 B CN101592644 B CN 101592644B
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Abstract
The invention discloses a method for detecting barium ions in oil field water. The method comprises the following steps: taking an oil-water sample; adding hydrochloric acid solution and methyl red indicator into the sample; adjusting the solution to yellow by ammonia solution; adding acetic acid-ammonium acetate buffer solution into the mixture; heating and boiling the mixture; dripping potassium chromate solution into the mixture; boiling the mixture once more; adding the acetic acid-ammonium acetate buffer solution into the mixture; standing the mixture to room temperature; filtering and abandoning initial filtrate; taking the filtrate; adding distilled water into the filtrate; adding potassium iodide and sulfuric acid solution into the mixture; shaking the mixture evenly, and placing the mixture in a dark position; titrating the mixture by sodium thiosulfate standard solution; adding starch indicating solution into the mixture; recording consumption V of the sodium thiosulfate solution; and calculating the concentration of the barium ions in the oil field through the formula of the consumption V0 of the recorded sodium thiosulfate solution. By adopting the method for detectingthe barium ions, the concentration of the barium ions in the oil field can be accurately and precisely detected, and the requirement of quick and accurate analysis on scaling ions Ba<2+> can be met.
Description
Technical field
The invention belongs to oil gas descalling technique field, be specifically related to the assay method of barium ion in a kind of oil-field water.
Background technology
Contain Ba in the output water of oil field
2+, take medicament antiscale measure at present, need monitoring medicament antiscaling effect, be carried out to incrustation ion analysis and mensuration.Ba
2+Analytical approach compleximetry, chromate volumetric method, iodimetric titration, gravimetric method, the chromatography of ions and atomic absorption spectrophotometry etc. are generally arranged.These traditional analysis determining method rig-site utilization still have some shortcomings, and are loaded down with trivial details as at least 6 hours consuming time of compleximetry, analytical procedure, mensuration be Ba
2+And Sr
2+Total amount, and only be applicable to the mensuration of content greater than the 100mg/l barium ion; About 15 hours consuming time of chromate volumetric method, analytical procedure is not only loaded down with trivial details, and is consuming time, power consumption is more, and operate miss is bigger, also only is applicable to Ba in the water
2+Content is greater than the mensuration of 100mg/L; Gravimetric method is for Ba
2+Have good selectivity, with high accuracy, but time-consuming, bothersome, need the accurate suction filtration device of a cover, and controlled stronger, blank test is failed easily; Iodimetric titration is adapted to Ba
2+The higher sample of content is measured, but the acidity of control is too strong, and the barium chromate of generation decomposes easily, causes than mistake; The chromatography of ions, atomic absorption spectrophotometry belong to instrumental method, this several method instrument costliness, and the preparation process of sample is loaded down with trivial details, is fit to measure the Ba of low concentration
2+
Summary of the invention
The objective of the invention is to solve low, the slow-footed problem of accuracy rating of tests when barium ion is measured in the oil-field water, provide a kind of process simple, easy to operate, can quick and precisely measure the method for testing of barium ion at the scene.
The technical solution adopted in the present invention is, the assay method of barium ion in the oil-field water specifically carries out according to following steps,
Step 1 is prepared reagent, and it is pure that following reagent is analysis:
1: 1 hydrochloric acid solution: the hydrochloric acid of every 100ml adds the distilled water diluting of 100ml;
2% ammonium acetate solution: every 2g ammonium acetate add 100ml dissolved in distilled water;
1% starch indicator solution: every 1g soluble starch add 100ml dissolved in distilled water;
The 25g/L potassium chromate solution: every 2.5g potassium chromate add 100ml dissolved in distilled water;
0.01mol/L hypo solution;
1: 15 sulfuric acid solution: the concentrated sulphuric acid of per 1 volume adds the distilled water of 15 volumes;
Acetate-ammonium acetate buffer solution of pH=5.9;
EDTA-Ca solution;
The ammonia spirit of pH=10;
Methyl red indicator;
Potassium iodide;
Red fuming nitric acid (RFNA);
Step 2, the test solution pre-service:
A. get the profit water sample as test solution;
B. be that filter media is fallen the suspension in the test solution with carbon black powders;
C. clear up reducing substances and organic contamination in the test solution with red fuming nitric acid (RFNA): add the 5.0ml red fuming nitric acid (RFNA) at every 100ml water sample, place on the electric hot plate and under the state that closely boils, the test solution steaming of step 1 is done near; Also coloured as solution, add 5.0ml nitric acid again, repeat aforesaid operations, limpid to solution; Be diluted with water to again about 10ml, with the ammonia spirit neutrality that neutralizes;
D. measure iron, aluminum ions content: if iron, aluminum ions content should be removed ferric ion and aluminium ion more than or equal to 1.0mg/L in the test solution after the c step handles; Shelter lead ion with EDTA-Ca solution;
Step 3, the pretreated test solution 10ml of the step 2 of learning from else's experience, this volume number is counted V
2, place triangular flask, add 2 hydrochloric acid solutions, add 100ml distilled water again, add the 0.1ml methyl red indicator, solution shows pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate-ammonium acetate buffer solution;
Step 4 adds several beaded glasses in triangular flask, heats on electric furnace, after boiling, drips the 10ml potassium chromate solution under constantly stirring;
Step 5, boil 3min again after, add 5ml acetate-ammonium acetate buffer solution while hot and shake up, on electric furnace, leave standstill room temperature, with ammonium acetate solution washing triangular flask 3 times, constant volume after shaking up, filters with quantitative filter paper at a slow speed, and discards initial filtrate in the 250ml volumetric flask;
Step 6 places iodine flask with the filtrate 10ml after 5 processing of transfer pipet removing step, and this volume number is counted V
1Adding distil water 100ml adds the 2g potassium iodide, the 10ml sulfuric acid solution, after shaking up, place 10min in the dark place, take out iodine flask with distilled water flushing bottle stopper and bottle wall, with the sodium thiosulfate standard solution titration, when solution is faint yellow, add 1.0ml starch indicator solution, titration to light green color is a terminal point, the consumption V of record hypo solution;
Step 7 is done blank test; Get distilled water 10ml and place triangular flask, add 2 hydrochloric acid solutions, add 100ml distilled water again, add the 0.1ml methyl red indicator, solution shows pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate-ammonium acetate buffer solution; Carry out the consumption V of record hypo solution again by above-mentioned steps 4,5,6
0
Step 8 is calculated Ba
2+
[Ba
2+]=[NC
Sulfo-(V
0-V) * 5.77/V
1] * 10
3
In the formula, C
Sulfo-Be the concentration of sodium thiosulfate, unit is mol/L;
N is extension rate 250/V
2
V
2Be the test solution volume of being got in the step 3, unit is ml;
V
1Be the filtrate volume of being got in the step 6, unit is ml;
V
0Be the volume of blank test consumption hypo solution, unit is ml;
V is the volume that sample consumes hypo solution, and unit is ml;
Promptly finish the mensuration of barium ion in the oil-field water.
Adopt barium ion assay method of the present invention, the concentration of barium ion in the test oil water in field that can be accurate, accurate, service condition is simple, operation is quick, is fit to the production scene to incrustation ion Ba
2+Fast, the needs accurately analyzed, make at the scene to more accurate on the use amount of antisludging agent dosage.
Embodiment
The present invention is described in detail below by embodiment.
Barium ion measuring principle of the present invention: the Ba that contains in pH=5.7～6.1
2+In the medium, add excessive potassium chromate, Ba
2+With potassium chromate reaction generation barium chromate precipitation, unnecessary potassium chromate and potassium iodide reaction generate iodine, with the iodine of sodium thiosulfate standard solution titration generation; By same quadrat method, get the distilled water of same volume, add potassium chromate with upper volume, do blank test, the sodium thiosulfate standard solution volume differences that is consumed according to blank test and actual measurement, thus calculate Ba
2+Content, reaction equation is as follows:
Ba
2++CrO
4 2-→BaCrO
4↓ (1)
2CrO
4 2-+6I
-+16H
+→3I
2+2Cr
3 ++8H
2O (2)
I
2+2Na
2S
2O
3→2NaI+Na
2S
4O
6 (3)
The barium ion assay method is specifically implemented according to following steps among the present invention:
Step 1 is prepared reagent, and it is pure that following reagent is analysis:
1: 1 hydrochloric acid solution: the hydrochloric acid of every 100ml adds the distilled water diluting of 100ml;
2% ammonium acetate solution: every 2g ammonium acetate add 100ml dissolved in distilled water;
1% starch indicator solution: every 1g soluble starch add 100ml dissolved in distilled water;
The 25g/L potassium chromate solution: every 2.5g potassium chromate add 100ml dissolved in distilled water;
0.01mol/L hypo solution;
1: 15 sulfuric acid solution: the concentrated sulphuric acid of per 1 volume adds the distilled water of 15 volumes;
Acetate-ammonium acetate buffer solution of pH=5.9;
EDTA-Ca solution;
The ammonia spirit of pH=10;
Methyl red indicator;
Potassium iodide;
Red fuming nitric acid (RFNA);
Step 2, sample pretreatment:
A. get the profit water sample as test solution;
B. be that filter media is fallen the suspension in the test solution with carbon black powders;
C. clear up reducing substances and organic contamination in the test solution with red fuming nitric acid (RFNA): add the 5.0ml red fuming nitric acid (RFNA) at every 100ml water sample, place on the electric hot plate and under the state that closely boils, sample is steamed near dried; Also coloured as solution, add 5.0ml nitric acid again, repeat aforesaid operations, limpid to solution; Be diluted with water to again about 10ml, with the ammonia spirit neutrality that neutralizes;
D. measure iron, aluminum ions content: if iron, aluminum ions content should be removed ferric ion and aluminium ion more than or equal to 1.0mg/L in the test solution; Shelter lead ion with EDTA-Ca solution;
Step 3, pretreated sample V learnt from else's experience
210ml places triangular flask, adds 2 hydrochloric acid solutions, adds 100ml distilled water again, adds the 0.1ml methyl red indicator, and solution should show pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate ammonium acetate buffer solution;
Step 4 adds several beaded glasses in triangular flask, heats on electric furnace, after boiling, drips the 10ml potassium chromate solution under constantly stirring;
Step 5, boil 3min again after, add 5ml acetate-ammonium acetate buffer solution while hot and shake up, on electric furnace, leave standstill room temperature, with ammonium acetate solution washing triangular flask 3 times, constant volume after shaking up, filters with quantitative filter paper at a slow speed, and discards initial filtrate in the 250ml volumetric flask;
Step 6 pipettes filtrate V with transfer pipet
110ml places iodine flask, adding distil water 100ml adds the 2g potassium iodide, the 10ml sulfuric acid solution, after shaking up, place 10min in the dark place, take out iodine flask with distilled water flushing bottle stopper and bottle wall, with the sodium thiosulfate standard solution titration, when solution is faint yellow, add 1.0ml starch indicator solution, titration to light green color is a terminal point, the consumption V of record hypo solution;
Step 7 is done blank test; Get distilled water 10ml and place triangular flask, add 2 hydrochloric acid solutions, add 100ml distilled water again, add the 0.1ml methyl red indicator, solution should show pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate ammonium acetate buffer solution; Carry out the consumption V of record hypo solution again by above-mentioned steps 4,5,6
0
Step 8 is calculated Ba
2+
[Ba
2+]=[NC
Sulfo-(V
0-V) * 5.77/V
1] * 10
3
In the formula, C
Sulfo-Be the concentration of sodium thiosulfate, unit is mol/L;
N is extension rate (250/V
2);
V
2Be the volume of sample of getting processing, unit is ml;
V
1By being got the filtrate volume number, unit is ml;
V
0Be the volume of blank test consumption hypo solution, unit is ml;
V is the volume that sample consumes hypo solution, and unit is ml;
Promptly finish the mensuration of barium ion in the oil field.
Can determine the adding concentration and the addition of antisludging agent according to the concentration of survey barium ion then, solve the inaccurate problem of on-the-spot dosage.
The quality index requirement
Ba wherein
2+The parallel analysis result should meet the quality requirements of table 1.
Table 1 Ba
2+Content range and analysis result requirement
| Ba 2+Content range/mg-L -1 | Relative deviation/% |
| ＜100 | 10.0 |
| 100～500 | 8.0 |
| ＞500～1000 | 4.0 |
| ＞1000～3000 | 2.0 |
In order to verify that indirect iodimetric titration of the present invention tests the accuracy of barium ion, the solution (accurately to 0.0002g) of the following 3 kinds of concentration known of preparation is made sample earlier: the A:100mg/L barium chloride solution; The B:660mg/L barium chloride solution; The lime chloride of C:1.0g/L, the magnesium chloride of 0.5g/L, 0.6g/L strontium chloride, 0.5g/L barium chloride mixed solution.Arrange first, second, the third 3 laboratory technicians to analyze A, B, C solution by above-mentioned analytical procedure then; After making parallel sample, average, analysis result sees Table 2 respectively, table 3.From table 2, table 3 as can be seen, indirect iodometric determination Ba of the present invention
2+, measured value is all in the error allowed band, to Ba
2+Have good selectivity, and this method of different tests person user is when analyzing, average relative error is also in the error allowed band.
Table 2 assay method analysis preparation of the present invention contains Ba
2+Coupon results
| Specimen coding | Actual value/mg-L -1 | Measured value/mg-L -1 | Relative error/% |
| A | 56.2 | 54.8 | -2.5 |
| Specimen coding | Actual value/mg-L -1 | Measured value/mg-L -1 | Relative error/% |
| B | 371.1 | 368.2 | -0.78 |
| C | 281.1 | 278.4 | -0.96 |
Table 3 different tests person analyzes the Ba that contains of preparation
2+Coupon results
Indirect iodimetric titration and existing gravimetric method, compleximetry, the iodimetric titration measurement result of the present invention being measured barium ion compare: with the Ba in the distinct methods analysis C sample
2+Content the results are shown in Table 4.As can be seen from Table 4, method relative error minimum of the present invention is also near actual value.
The different analytical results of table 4 relatively
| The method classification | Ba 2+Analysis result/mg-L -1 | Relative error/% |
| Actual value | 281.1 | |
| Gravimetric method | 251.2 | -10.6 |
| Compleximetry | 269.1 | -4.3 |
| Iodimetric titration | 262.2 | -6.7 |
| Indirect iodimetric titration | 278.4 | -0.96 |
At the field produces scene, the dosage of antisludging agent depend on incrustation ion content what, so that incrustation ion is accurately measured is most important 5,, can not reflect truth if the resultant error that analyzes is very big, can't solve on-the-spot problem.By Ba of the present invention
2+Analytical approach just can obtain the real content of the incrustation ion of each point, provides reliable data for determining suitable antisludging agent dosage.No matter and in the past should station incrustation ion content what, each meter is joined the antisludging agent that the station all adds same amount, has so both wasted many antisludging agents, total scale inhibition effect also bad, have only 50.1%.After adopting new method of the present invention, each meter is joined the incrustation ion content at station and analyze, and redefined the amount of antisludging agent according to different separately content.Compare now with in the past, can save a large amount of antisludging agents every day, and total scale inhibition effect has improved 12.4%.After total scale inhibition effect improved, pipeline and big jar amount of scale buildup reduced, and have prolonged the pipeline operating period, reduce clear jar number of times, and its economic benefit is very remarkable.
Claims (1)
1. the assay method of barium ion in the oil-field water is characterized in that, specifically carries out according to following steps:
Step 1 is prepared reagent, and it is pure that following reagent is analysis:
1: 1 hydrochloric acid solution: the hydrochloric acid of every 100ml adds the distilled water diluting of 100ml;
2% ammonium acetate solution: every 2g ammonium acetate add 100ml dissolved in distilled water;
1% starch indicator solution: every 1g soluble starch add 100ml dissolved in distilled water;
The 25g/L potassium chromate solution: every 2.5g potassium chromate add 100ml dissolved in distilled water;
0.01mol/L hypo solution;
1: 15 sulfuric acid solution: the concentrated sulphuric acid of per 1 volume adds the distilled water of 15 volumes;
Acetate-ammonium acetate buffer solution of pH=5.9;
EDTA-Ca solution;
The ammonia spirit of pH=10;
Methyl red indicator;
Potassium iodide;
Red fuming nitric acid (RFNA);
Step 2, the test solution pre-service:
A. get the profit water sample as test solution;
B. be that filter media is fallen the suspension in the test solution with carbon black powders;
C. clear up reducing substances and organic contamination in the test solution with red fuming nitric acid (RFNA): add the 5.0ml red fuming nitric acid (RFNA) at every 100ml water sample, place on the electric hot plate and under the state that closely boils, the test solution steaming of step 1 is done near; Also coloured as solution, add 5.0ml nitric acid again, repeat aforesaid operations, limpid to solution; Be diluted with water to again about 10ml, with the ammonia spirit neutrality that neutralizes;
D. measure iron, aluminum ions content: if iron, aluminum ions content should be removed ferric ion and aluminium ion more than or equal to 1.0mg/L in the test solution after the c step handles; Shelter lead ion with EDTA-Ca solution;
Step 3, the pretreated test solution 10ml of the step 2 of learning from else's experience, this volume number is counted V
2, place triangular flask, add 2 hydrochloric acid solutions, add 100ml distilled water again, add the 0.1ml methyl red indicator, solution shows pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate-ammonium acetate buffer solution;
Step 4 adds several beaded glasses in triangular flask, heats on electric furnace, after boiling, drips the 10ml potassium chromate solution under constantly stirring;
Step 5, boil 3min again after, add 5ml acetate-ammonium acetate buffer solution while hot and shake up, on electric furnace, leave standstill room temperature, with ammonium acetate solution washing triangular flask 3 times, constant volume after shaking up, filters with quantitative filter paper at a slow speed, and discards initial filtrate in the 250ml volumetric flask;
Step 6 places iodine flask with the filtrate 10ml after 5 processing of transfer pipet removing step, and this volume number is counted V
1Adding distil water 100ml adds the 2g potassium iodide, the 10ml sulfuric acid solution, after shaking up, place 10min in the dark place, take out iodine flask with distilled water flushing bottle stopper and bottle wall, with the sodium thiosulfate standard solution titration, when solution is faint yellow, add 1.0ml starch indicator solution, titration to light green color is a terminal point, the consumption V of record hypo solution;
Step 7 is done blank test; Get distilled water 10ml and place triangular flask, add 2 hydrochloric acid solutions, add 100ml distilled water again, add the 0.1ml methyl red indicator, solution shows pink, uses the ammonia spirit regulator solution again to yellow, adds 10ml acetate-ammonium acetate buffer solution; Carry out the consumption V of record hypo solution again by above-mentioned steps 4,5,6
0
Step 8 is calculated Ba
2+
[Ba
2+]=[NC
Sulfo-(V
0-V) * 45.77/V
1] * 10
3
In the formula, C
Sulfo-Be the concentration of sodium thiosulfate, unit is mol/L;
N is extension rate 250/V
2
V
2Be the test solution volume of being got in the step 3, unit is ml;
V
1Be the filtrate volume of being got in the step 6, unit is ml;
V
0Be the volume of blank test consumption hypo solution, unit is ml;
V is the volume that sample consumes hypo solution, and unit is ml;
Promptly finish the mensuration of barium ion in the oil-field water.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103037702A CN101592644B (en) | 2009-06-27 | 2009-06-27 | Method for detecting barium ions in oil field water |
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| CN101592644B true CN101592644B (en) | 2010-09-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102175746B (en) * | 2010-12-30 | 2013-08-07 | 株洲冶炼集团股份有限公司 | Analytical reagent and method for analyzing content of sulfuric acid and ferric irons |
| CN105403678A (en) * | 2015-10-28 | 2016-03-16 | 陕西省石油化工研究设计院 | Method for evaluating scaling trend of oil field water |
| CN107064129A (en) * | 2017-04-27 | 2017-08-18 | 西安石油大学 | A kind of oil field underwater gold belongs to cation quick quantitative analytic method |
Citations (2)
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|---|---|---|---|---|
| US5270216A (en) * | 1992-02-13 | 1993-12-14 | Gas Research Institute | Measurement of low phosphonate concentrations |
| CN101046453A (en) * | 2007-04-24 | 2007-10-03 | 青海西部矿业科技有限公司 | Iodometry process of measuring gold content in high accuracy and precision |
-
2009
- 2009-06-27 CN CN2009103037702A patent/CN101592644B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5270216A (en) * | 1992-02-13 | 1993-12-14 | Gas Research Institute | Measurement of low phosphonate concentrations |
| CN101046453A (en) * | 2007-04-24 | 2007-10-03 | 青海西部矿业科技有限公司 | Iodometry process of measuring gold content in high accuracy and precision |
Non-Patent Citations (2)
| Title |
|---|
| 吴卫东.掩蔽锶-铬酸钡-碘量法测定碳酸锶中钡.《无机盐工业》.2000,第32卷(第5期),45-47. * |
| 唐光锡.重铬酸钾容量法测定重晶石、煅料和煅料浸取液中钡.《井矿盐技术》.1987,(第73期),14-18. * |
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