CN107064129A - A kind of oil field underwater gold belongs to cation quick quantitative analytic method - Google Patents
A kind of oil field underwater gold belongs to cation quick quantitative analytic method Download PDFInfo
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Abstract
A kind of oil field underwater gold belongs to cation quick quantitative analytic method, using compleximetry, on the premise of to sample without special pre-treatment, by controlling the acidity and precipitation masking method of solution to realize the stepwise titration to calcium in the water sample of oil field, magnesium, strontium, barium and iron, due to reducing the step of removing iron, heating, ageing, filtering and dilute, so as to greatly reduce operating procedure and time, increase the degree of accuracy of measurement result, operating efficiency is improved, this method is expected to be widely applied in the water analysis of oil field.
Description
Technical field
The present invention relates to oil field water analysis field, and in particular to a kind of oil field underwater gold belongs to cation fast quantitative analysis
Method.
Background technology
In oilfield development process, with the extension of development time, strata pressure is gradually reduced, therefore passes through special note
Enter well and inject water into oil reservoir, keep or recover formation pressure, oil reservoir is had very strong driving force, be the exploitation rate for improving oil reservoir
With an important means of recovery ratio and measure.Then, because injection water source is general complex, including oil well produced water,
Zwitterion content in table water, shallow seated groundwater etc., these separate sources water is also different, especially calcium, magnesium, strontium, barium, iron etc.
Incrustation ion etc., if detected before injection without analysis, and passes through proper treatment, then injection water can be caused to be tied in oil reservoir
Dirt, blocks stratum, finally has a strong impact on waterflooding development effect.Therefore, oil field water analysis is particularly important, and is also oil field note
An important process in water development process.
Mainly there is traditional compleximetry and modern instrumental analysis method for the measure of oil field water cationic, including
Chromatography of ions and atom spectrum etc., wherein compleximetry belong to macro-analysis, and the degree of accuracy is higher, and chromatography of ions and atom light
Spectrum belongs to micro/trace analysis, although sensitivity is very high, but the degree of accuracy is relatively low, therefore, and current oil field water sample analysis are generally adopted
It is mainly oil and gas industry standard ST/T 5329-94 with the standard of foundation with traditional compleximetry《Chip shale oil
Hide injection water quality fertilizer index and analysis method》(hereinafter referred to as professional standard), but these methods generally deposit in measurement process
Except iron, heating, place the operations such as ageing, filtering, dilution, not only troublesome poeration, time long and excessive step causes to survey
Error increase is measured, this is also common problem in current oil field water water analysis.
The content of the invention
In order to overcome the shortcoming of above-mentioned prior art, belong to cation it is an object of the invention to provide a kind of oil field underwater gold
Quick quantitative analytic method, reduces operating procedure and time, improves the degree of accuracy of measurement result, improves operating efficiency.
In order to achieve the above object, the present invention is adopted the technical scheme that：
A kind of oil field underwater gold belongs to cation quick quantitative analytic method, comprises the following steps：
1) oil field 5~50mL of water sample is pipetted with pipette in 250mL conical flasks, volume is designated as V0, plus distilled water is to total
Volume is 50mL, then adds 10mL, 0.1mol/L salpeter solution and 2 drops 0.2% xylenol orange indicator, uses
0.01mol/L EDTA standard liquids are titrated to solution and are changed into brownish red from aubergine, then the xylenol orange for drop 0.2% of Jia 1 refers to
Show agent, sport glassy yellow, as terminal, record the EDTA of consumption volume (mL) V1If, V1Less than 2mL, then increase V0's
Amount, if V1More than 20mL, then reduce V0Amount；Finally according to V1Calculate the total amount tapped a blast furnace；
2) in step 1) NaOH solution that mass concentration is 4%, the pH value of regulation to solution is added dropwise in the solution that titrated
For 3~4,5mL is then added, mass concentration is 10% ammonium sulfate, and stirring makes the strontium barium in water sample precipitate completely, adds
Absolute ethyl alcohol 2mL suppresses precipitation dissolving, adds the NH that mass concentration is 10%3-NH4Cl cushioning liquid makes its pH=10, with chromium
Black T is indicator, and solution is titrated to 0.01mol/L EDTA standard liquids and is changed into pure blue from claret, record consumption
EDTA volumes (mL) V2, according to V2Calculate the total amount of calcium and magnesium in water sample；
3) in step 2) titrate in the solution completed and continue plus 10mL, 4% sodium hydroxide solution, then add the instruction of 3mg calcium
Agent, it is terminal that pure blue is dropped to EDTA standard liquids, and EDTA standard liquids consumption (mL) is denoted as V3, according to V3Calculate calcium
Content；
4) a V is pipetted again with pipette in addition0ML water sample is in conical flask, and adding water makes cumulative volume be 50mL, plus
10mL10% NH3-NH4Cl cushioning liquid, 3~4 drop chromium black T indicators, is dropped to pure with 0.01mol/L EDTA standard liquids
Blueness is terminal, and EDTA standard liquids consumption (mL) is denoted as V4, according to V4Calculate the total amount of calcium and magnesium strontium barium；
5) content is calculated：
Analysis principle：In the acid solution of pH2~3, metal iron ion can form stable complex compound with EDTA, and
Other metal ions can not then form stable complex compound, Er Qie because EDTA Radiation grafting and Complex Stability Constants are relatively low
Expose in the presence of oxygen and nitric acid, the iron ion in water sample all exists in ferric form, therefore in 0.1mol/L acid solution
Only titrate total iron.
When pH is increased to 3~4, adding ammonium sulfate can be such that barium and strontium in sample precipitates completely, and the addition of ethanol can press down
System precipitation dissolving, when pH value of solution is increased to 10 or so, the iron ion in solution is also completely with Fe (OH)3The form of precipitation is deposited
, therefore the total content of magnesium and calcium is titrated with EDTA, it can use EDTA titration of calcium ions when continuing and increasing pH to 12.
A water sample is separately taken, regulation pH value is 10, and the total amount of calcium and magnesium strontium barium is determined with EDTA.Beneficial effects of the present invention
For：
(1) present invention is handled when determining calcium and magnesium strontium barium without except iron, because iron ion is in pH=10 buffer solution
Precipitation is complete, without interference with other ion measurements；
(2) measure of iron ion is carried out in the salpeter solution of pH=2~3, and only iron ion can be with this condition
EDTA is complexed, therefore can individually determine the total amount of iron；
(3) barium and strontium are precipitated complete with ammonium sulfate in the case where pH is 3~4 acid condition, and pressed down using ethanol is added
Make precipitation dissolving, then by pH be transferred to 10 with EDTA titrate the total content of magnesium and calcium, without will precipitation by heating, place ageing,
The operation such as filtering and dilution constant volume, greatly reduces operating procedure, saves the operating time.
(4) measure of iron ion and calcium ions and magnesium ions can be carried out in a solution.
(5) invention determines the calcium and magnesium strontium barium and iron ion degree of accuracy height in the water sample of oil field, favorable reproducibility.
The present invention uses compleximetry, on the premise of to sample without special pre-treatment, by controlling solution
Acidity and precipitation masking method realize the stepwise titration to calcium in the water sample of oil field, magnesium, strontium, barium and iron, due to reduce remove iron plus
The step of heat, ageing, filtering and dilution, so as to greatly reduce operating procedure and time, increase the degree of accuracy of measurement result, improve
Operating efficiency, this method is expected to be widely applied in the water analysis of oil field.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of oil field underwater gold of embodiment belongs to cation quick quantitative analytic method, comprises the following steps：
1) oil field water sample 10mL is pipetted with pipette in 250mL conical flasks, plus distilled water to cumulative volume is 50mL, then
10mL, 0.1mol/L salpeter solution and 2 drops 0.2% xylenol orange indicator are added, it is molten with 0.01mol/L EDTA standards
Liquid is titrated to solution and is changed into brownish red from aubergine, then drop 0.2% of Jia 1 xylenol orange indicator, sport glassy yellow, be
Terminal, the volume for recording the EDTA of consumption is 2.45mL；
2) in step 1) NaOH solution that mass concentration is 4% is added dropwise in the solution that titrated, it is adjusted to the pH value of solution
For 3~4,5mL is then added, mass concentration is 10% ammonium sulfate, is sufficiently stirred for making the strontium barium in water sample to precipitate completely,
Add absolute ethyl alcohol 2mL and suppress precipitation dissolving, add the NH that mass concentration is 10%3-NH4Cl cushioning liquid makes its pH=10,
Using eriochrome black T as indicator, it is titrated to solution with 0.01mol/L EDTA standard liquids and pure blue is changed into from claret, accurate note
Record the EDTA volumes 18.24mL of consumption；
3) in step 2) titrate in the solution completed and continue plus 10mL, 4% sodium hydroxide solution, then add the instruction of 3mg calcium
Agent, it is terminal that pure blue is dropped to EDTA standard liquids, and EDTA standard liquids consumption is 9.58mL；
4) a 10mL water sample is pipetted again with pipette in conical flask in addition, plus distilled water makes the cumulative volume be
50mL, plus 10mL10% NH3-NH4Cl cushioning liquid, 3~4 drop chromium black T indicators, with 0.01mol/L EDTA standard liquids
Pure blue is dropped to for terminal, EDTA standard liquids consumption is 19.36mL；
5) content is calculated：Total iron is 136.81mg/L, and calcium content is 383.97mg/L, and content of magnesium is 210.44mg/L, strontium
Barium content is 153.82mg/L.
The rate of recovery is tested：
Example water sample 1L, is then respectively adding 99.2mg ferric ion, 100.5mg calcium ions, 101.4mg magnesium
Ion and 98.9mg barium ions, stirring fully dissolving after take 10mL water samples to be analyzed with pipette, analytical procedure with example 1,
Measurement result is shown in Table 1：
From rate of recovery experimental result can be seen that using this method measure the rate of recovery of result 94.76%~
Between 106.82%, it is fully able to meet requirement of the field assay to error.
Claims (2)
1. a kind of oil field underwater gold belongs to cation quick quantitative analytic method, it is characterised in that comprise the following steps：
1) oil field 5~50mL of water sample is pipetted with pipette in 250mL conical flasks, volume is designated as V0, plus distilled water to cumulative volume is
50mL, then adds 10mL, 0.1mol/L salpeter solution and 2 drops 0.2% xylenol orange indicator, with 0.01mol/L's
EDTA standard liquids are titrated to solution and are changed into brownish red from aubergine, then drop 0.2% of Jia 1 xylenol orange indicator, sport
Glassy yellow, as terminal, record the EDTA of consumption volume (mL) V1If, V1Less than 2mL, then increase V0Amount, if V1Greatly
In 20mL, then reduce V0Amount；Finally according to V1Calculate the total amount tapped a blast furnace；
2) in step 1) be added dropwise the NaOH solution that mass concentration is 4% in the solution that titrated, the pH value of regulation to solution for 3~
4,5mL is then added, mass concentration is 10% ammonium sulfate, and stirring makes the strontium barium in water sample precipitate completely, adds anhydrous
Ethanol 2mL suppresses precipitation dissolving, adds the NH that mass concentration is 10%3-NH4Cl cushioning liquid makes its pH=10, with eriochrome black T
For indicator, solution is titrated to 0.01mol/L EDTA standard liquids pure blue is changed into from claret, record the EDTA of consumption
Volume (mL) V2, according to V2Calculate the total amount of calcium and magnesium in water sample；
3) in step 2) titrate in the solution completed and continue plus 10mL, 4% sodium hydroxide solution, then add 3mg calcon-carboxylic acids, use
EDTA standard liquids drop to pure blue for terminal, and EDTA standard liquids consumption (mL) is denoted as V3, according to V3Calculate the content of calcium；
4) a V is pipetted again with pipette in addition0ML water sample is in conical flask, and adding water makes cumulative volume be 50mL, plus
10mL10% NH3-NH4Cl rushes solution, and 3~4 drop chromium black T indicators drop to ethereal blue with 0.01mol/L EDTA standard liquids
Color is terminal, and EDTA standard liquids consumption (mL) is denoted as V4, according to V4Calculate the total amount of calcium and magnesium strontium barium；
5) content is calculated：
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2. a kind of oil field underwater gold according to claim 1 belongs to cation quick quantitative analytic method, it is characterised in that bag
Include following steps：
1) oil field water sample 10mL is pipetted with pipette in 250mL conical flasks, plus distilled water to cumulative volume is 50mL, is then added
The xylenol orange indicator of 10mL, 0.1mol/L salpeter solution and 2 drops 0.2%, is dripped with 0.01mol/L EDTA standard liquids
It is fixed to be changed into brownish red to solution from aubergine, then drop 0.2% of Jia 1 xylenol orange indicator, sport glassy yellow, be end
Point, the volume for recording the EDTA of consumption is 2.45mL；
2) in step 1) NaOH solution that mass concentration is 4% is added dropwise in the solution that titrated, be adjusted to the pH value of solution for 3~
4,5mL is then added, mass concentration is 10% ammonium sulfate, is sufficiently stirred for making the strontium barium in water sample to precipitate completely, is added
Absolute ethyl alcohol 2mL suppresses precipitation dissolving, adds the NH that mass concentration is 10%3-NH4Cl cushioning liquid makes its pH=10, with chromium
Black T is indicator, is titrated to solution with 0.01mol/L EDTA standard liquids and is changed into pure blue from claret, accurate recording disappears
The EDTA volumes 18.24mL of consumption；
3) in step 2) titrate in the solution completed and continue plus 10mL, 4% sodium hydroxide solution, then add 3mg calcon-carboxylic acids, use
EDTA standard liquids drop to pure blue for terminal, and EDTA standard liquids consumption is 9.58mL；
4) a 10mL water sample is pipetted again with pipette in addition in conical flask, plus distilled water makes cumulative volume be 50mL, plus
10mL10% NH3-NH4Cl cushioning liquid, 3~4 drop chromium black T indicators, is dropped to pure with 0.01mol/L EDTA standard liquids
Blueness is terminal, and EDTA standard liquids consumption is 19.36mL；
5) content is calculated：Total iron is 136.81mg/L, and calcium content is 383.97mg/L, and content of magnesium is 210.44mg/L, and strontium barium contains
Measure as 153.82mg/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918753A (en) * | 2018-07-11 | 2018-11-30 | 中国科学院青海盐湖研究所 | The measuring method of content of strontium in al-sr alloy |
| CN108956852A (en) * | 2018-07-05 | 2018-12-07 | 中国石油天然气股份有限公司 | A kind of evaluation method of oil field high-content barium sulfate scale antisludging agent scale inhibition performance |
| CN109374818A (en) * | 2018-10-29 | 2019-02-22 | 中国海洋石油集团有限公司 | Quickly device and method of the measurement complexing agent to complexing of metal ion ability |
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| CN102507573A (en) * | 2011-11-17 | 2012-06-20 | 王慧屏 | Method for measuring content of calcium ions in oil field water |
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| CN101592644A (en) * | 2009-06-27 | 2009-12-02 | 延长油田股份有限公司吴起采油厂 | The assay method of barium ion in the oil-field water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956852A (en) * | 2018-07-05 | 2018-12-07 | 中国石油天然气股份有限公司 | A kind of evaluation method of oil field high-content barium sulfate scale antisludging agent scale inhibition performance |
| CN108918753A (en) * | 2018-07-11 | 2018-11-30 | 中国科学院青海盐湖研究所 | The measuring method of content of strontium in al-sr alloy |
| CN109374818A (en) * | 2018-10-29 | 2019-02-22 | 中国海洋石油集团有限公司 | Quickly device and method of the measurement complexing agent to complexing of metal ion ability |
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