CN103234965B - The detection method of KCE content in activated water fracturing fluid - Google Patents
The detection method of KCE content in activated water fracturing fluid Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000012530 fluid Substances 0.000 title claims abstract description 99
- 238000001514 detection method Methods 0.000 title claims abstract description 35
- -1 sodium tetraphenylborate Chemical compound 0.000 claims abstract description 206
- 239000012086 standard solution Substances 0.000 claims abstract description 183
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 133
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 111
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 111
- 239000001103 potassium chloride Substances 0.000 claims abstract description 65
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 65
- 238000004448 titration Methods 0.000 claims abstract description 56
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910001414 potassium ion Inorganic materials 0.000 claims abstract description 24
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 20
- 238000001556 precipitation Methods 0.000 claims abstract description 18
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 68
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 26
- 239000000706 filtrate Substances 0.000 claims description 20
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical group C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 claims description 18
- 239000000872 buffer Substances 0.000 claims description 16
- 238000010790 dilution Methods 0.000 claims description 16
- 239000012895 dilution Substances 0.000 claims description 16
- 239000007974 sodium acetate buffer Substances 0.000 claims description 15
- 230000000694 effects Effects 0.000 claims description 9
- 230000001376 precipitating effect Effects 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000010276 construction Methods 0.000 abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 230000003139 buffering effect Effects 0.000 description 6
- 238000003556 assay Methods 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003458 metachromatic effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- VADKRMSMGWJZCF-UHFFFAOYSA-N 2-bromophenol Chemical compound OC1=CC=CC=C1Br VADKRMSMGWJZCF-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002696 acid base indicator Substances 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 108700002783 roundabout Proteins 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses the detection method of KCE content in a kind of activated water fracturing fluid, the method includes: add certain volume and excessive sodium tetraphenylborate standard solution, the potassium ion in precipitation activated water fracturing fluid in the activated water fracturing fluid of certain volume；Then, add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；Quality according to the hydrocarbon ammonium salt in the hydrocarbon ammonium salt standard solution that titration uses, calculate the quality of the sodium tetraphenylborate reacted, obtain the quality of the sodium tetraphenylborate reacted with the potassium ion in activated water fracturing fluid, and then the ratio obtaining the of the fracturing fluid quality of activated water of the quality of potassium chloride in activated water fracturing fluid, the quality of this potassium chloride and described certain volume is the content of potassium chloride in this activated water fracturing fluid.Technical scheme result is accurate, easy and simple to handle, is not limited by instrument and equipment condition, it is possible to use at the construction field (site).
Description
Technical field
The present invention relates to mining construction field, particularly to the detection method of KCE content in activated water fracturing fluid.
Background technology
In the fracturing fluid of interior gasser, activated water fracturing fluid pollutes the feature such as little and is subject to extensive use because cost is low, residue content is few, to coal seam.In order to ensure construction quality, it is ensured that in fracturing fluid, the effective content of potassium chloride meets the requirement of design, the fracturing fluid that each construction team prepares need to be detected.Conventional detection method is to deliver in laboratory after being sampled by the fracturing fluid prepared, and adopts gravimetric method to carry out.Due to the method complex operation, time-consuming, the detection cycle needs 8-10 hour, and the method needs the experimental facilitiess such as thermostatic drying chamber, and job site cannot meet corresponding experiment condition, can only be sampled in laboratory and detect, so cause that testing result is delayed and be unfavorable for the on-the-spot quality control to construction material of pressing crack construction.
Summary of the invention
In view of the above problems, it is proposed that the present invention in case provide a kind of overcome the problems referred to above or solve the activated water fracturing fluid of the problems referred to above at least in part in the detection method of KCE content.
For reaching above-mentioned purpose, the technical scheme is that and be achieved in that:
The invention discloses the detection method of KCE content in a kind of activated water fracturing fluid, the method includes: add certain volume and excessive sodium tetraphenylborate standard solution, the potassium ion in precipitation activated water fracturing fluid in the activated water fracturing fluid of certain volume；Then, add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；Quality according to the hydrocarbon ammonium salt in the hydrocarbon ammonium salt standard solution that titration uses, calculate the quality of the sodium tetraphenylborate reacted, obtain the quality of the sodium tetraphenylborate reacted with the potassium ion in activated water fracturing fluid, and then the ratio obtaining the of the fracturing fluid quality of activated water of the quality of potassium chloride in activated water fracturing fluid, the quality of this potassium chloride and described certain volume is the content of potassium chloride in this activated water fracturing fluid.
In this activated water fracturing fluid, the detection method of KCE content also includes:
After the activated water fracturing fluid of certain volume adds buffer, add excessive sodium tetraphenylborate standard solution；
In this activated water fracturing fluid in the detection method of KCE content, described buffer is Acetic acid-sodium acetate buffer；
In this activated water fracturing fluid in the detection method of KCE content, indicator is bromophenol blue solution；With the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, it is titrated to corresponding color for the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, being titrated to blueness.
The invention also discloses the detection method of the content of potassium chloride in a kind of activated water fracturing fluid, the method includes:
Potassium chloride standard solution V7Milliliter, adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；Add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V1Milliliter, after precipitating completely by potassium ion, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution is V1Milliliter；
Take sodium tetraphenylborate standard solution X milliliter；Add described corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium normal saline solution that record titration uses is V0Milliliter；
Calculate the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；
Accurately pipetting the activated water fracturing fluid V milliliter filtered with dry filter paper, being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Take the activated water fracturing fluid V after dilution7Milliliter, adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；Add described corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V2Milliliter；In calculated activity water fracturing fluid, the content of potassium chloride is:Here, ρ is the of the fracturing fluid density of activated water of described V milliliter.
In this activated water fracturing fluid, the detection method of KCE content also includes:
At described potassium chloride standard solution V7After milliliter, add buffer further, add excessive sodium tetraphenylborate standard solution X milliliter；
Described take sodium tetraphenylborate standard solution X milliliter after；Add buffer further, then with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；
Described take dilution after activated water fracturing fluid V7After milliliter, after adding buffer further, add excessive sodium tetraphenylborate standard solution X milliliter.
In this activated water fracturing fluid in the detection method of KCE content, described buffer is that Acetic acid-sodium acetate cushions night；
In this activated water fracturing fluid in the detection method of KCE content, described indicator is bromophenol blue solution；Described it is titrated to corresponding color for being titrated to blueness.
The invention also discloses the detection method of KCE content in a kind of activated water fracturing fluid, the method includes:
Potassium chloride standard solution V7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to described V4The subsequent filtrate of milliliter adds corresponding indicator, with the sodium tetraphenylborate standard solution in subsequent filtrate described in hydrocarbon ammonium salt standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V5Milliliter；According to formulaCalculate V1, here, V1After precipitating the potassium chloride standard solution potassium ion taken completely, the volume of the hydrocarbon ammonium salt standard solution used when remaining sodium tetraphenylborate reacts with hydrocarbon ammonium salt standard solution；
Take sodium tetraphenylborate standard solution X milliliter；Add described corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium normal saline solution that record titration uses is V0Milliliter；
Calculate the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；
Accurately pipetting the activated water fracturing fluid V milliliter filtered with dry filter paper, being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Take the activated water fracturing fluid V after dilution7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to the V taken4The subsequent filtrate of milliliter adds corresponding indicator, with the sodium tetraphenylborate standard solution in hydrocarbon ammonium salt the taken subsequent filtrate of standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V6Milliliter；According to formulaCalculate V2, V here2After precipitating the potassium ion in the activated water fracturing fluid taken completely, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution；
In calculated activity water fracturing fluid, the content of potassium chloride is:Here, ρ is the of the fracturing fluid density of activated water of described V milliliter..
In this activated water fracturing fluid, the detection method of KCE content also includes:
At potassium chloride standard solution V7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in after, add further Acetic acid-sodium acetate buffer, then add excessive sodium tetraphenylborate standard solution X milliliter；
After taking sodium tetraphenylborate standard solution X milliliter, add Acetic acid-sodium acetate buffer further, then add corresponding indicator；
Activated water fracturing fluid V after taking dilution7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in after, add further Acetic acid-sodium acetate buffer, add excessive sodium tetraphenylborate standard solution X milliliter；
Described indicator is bromophenol blue solution, described in be titrated to corresponding color for being titrated to blueness.
Technical scheme result is accurate, easy and simple to handle, is not limited by instrument and equipment condition, it is possible to use at the construction field (site).
Accompanying drawing explanation
The detection method flow chart of KCE content in a kind of activated water fracturing fluid that Fig. 1 provides for the embodiment of the present invention；
The detection method flow chart of the content of potassium chloride in a kind of activated water fracturing fluid that Fig. 2 provides for further embodiment of this invention.
Detailed description of the invention
The core concept of the present invention is the detection method of KCE content in open activated water fracturing fluid, and the method includes: add certain volume and excessive sodium tetraphenylborate standard solution, the potassium ion in precipitation activated water fracturing fluid in the activated water fracturing fluid of certain volume；Then, add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；Quality according to the hydrocarbon ammonium salt in the hydrocarbon ammonium salt standard solution that titration uses, calculate the quality of the sodium tetraphenylborate reacted, obtain the quality of the sodium tetraphenylborate reacted with the potassium ion in activated water fracturing fluid, and then the ratio obtaining the of the fracturing fluid quality of activated water of the quality of potassium chloride in activated water fracturing fluid, the quality of this potassium chloride and described certain volume is the content of potassium chloride in this activated water fracturing fluid.
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
In an embodiment of the present invention, having used sodium tetraphenylborate standard solution, potassium chloride standard solution and hydrocarbon ammonium salt standard solution, Acetic acid-sodium acetate buffer, bromophenol blue solution, above-mentioned solution is prepared in laboratory.
The above-mentioned sodium tetraphenylborate standard solution that is previously mentioned refers to the certain density sodium tetraphenylborate solution configured, in other embodiments of the invention, sodium tetraphenylborate standard solution can also be the sodium tetraphenylborate solution of other concentration, in an embodiment of the present invention, the compound method of sodium tetraphenylborate standard solution is as follows: take sodium tetraphenylborate Na (C6H5)4B7.0 gram, the 50 milliliters of vibrations that add water make sodium tetraphenylborate dissolve, and add the aluminium hydroxide Al (OH) of new preparation3Gel, adds NaCl16.6 gram of sodium chloride, fully shakes up, and adds water 250 milliliters, jolting 15 minutes, stands 10 minutes, filters, and drips sodium hydroxide NaOH test solution to PH=8～9, add water and be diluted to 1000 milliliters, shake up in filtrate.Here, the compound method of above-mentioned gel aluminum hydroxide is as follows: take aluminum chloride AlCl31.0 grams.It is dissolved in 25 milliliters of water, under being stirred continuously, slowly drips sodium hydroxide solution to PH8～9.
The above-mentioned potassium chloride standard solution that is previously mentioned refers to the certain density Klorvess Liquid configured, in other embodiments of the invention, potassium chloride standard solution can also be the Klorvess Liquid of other concentration, in an embodiment of the present invention, the compound method of potassium chloride standard solution is as follows: accurately weigh 0.2 gram of benchmark potassium chloride (KCl) being dried to constant weight at 150 DEG C, it is dissolved in water and is placed in 250 milliliters of volumetric flasks, add water the full scale line place being diluted to volumetric flask, shake up.The density p of this potassium chloride standard solution can be calculated1=0.2g/250ml=0.0008g/ml.
The above-mentioned hydrocarbon ammonium salt standard solution being previously mentioned refers to the certain density hydrocarbon ammonium salt solution configured, in other embodiments of the invention, hydrocarbon ammonium salt standard solution can also be the hydrocarbon ammonium salt solution of other concentration, in an embodiment of the present invention, the compound method of hydrocarbon ammonium salt standard solution is as follows: take chlorodimethyl benzyl hydrocarbon ammonium 3.8 grams, after being dissolved in water, adds Acetic acid-sodium acetate buffer (PH=3.7 of Acetic acid-sodium acetate buffer) 10 milliliters, add water and be diluted to 1000 milliliters, shake up.Hydrocarbon ammonium salt mentioned above is a type organic matter, has multiple, and what this experiment adopted is chlorodimethyl benzyl hydrocarbon ammonium, it would however also be possible to employ other hydrocarbon ammonium salt, chlorodimethyl benzyl hydrocarbon ammonium is also named chlorination alkyl dimethyl for benzene potassium ammonium, benzalkonium chloride etc., and molecular formula is C21H38ClN, chemical structural formula is:
The compound method of Acetic acid-sodium acetate buffer is as follows: take anhydrous sodium acetate 20 grams, add water 300 milliliters after dissolving, add bromophenol blue indicator solution 1 milliliter and 60 milliliters～80 milliliters of glacial acetic acid, be changed into pure green to solution from blueness, add water and be diluted to 1000 milliliters, shake up.The pH value of preparation Acetic acid-sodium acetate buffer out is 3.7.
The compound method of bromophenol blue solution is as follows: take bromophenol blue 0.1 gram, adds 3 milliliters of bromophenol blues of 0.05 mol/L NaOH solution and dissolves, adds water and be diluted to 200 milliliters, shake up.
In an embodiment of the present invention, sodium tetraphenylborate in sodium tetraphenylborate standard solution can react with potassium chloride, activated water fracturing fluid and potassium chloride standard solution all there is potassium chloride, therefore chemical reaction can be there is when adding sodium tetraphenylborate standard solution in standard chlorination potassium solution, chemical reaction can be there is when adding sodium tetraphenylborate standard solution in activated water fracturing fluid；Sodium tetraphenylborate in sodium tetraphenylborate standard solution can also react with the hydrocarbon ammonium salt in hydrocarbon ammonium salt standard solution, and hydrocarbon ammonium salt refers to chlorodimethyl benzyl hydrocarbon ammonium here.
Sodium tetraphenylborate is as follows with the chemical equation of potassium chloride:
Na(C6H5)4B+KCl→K(C6H5)4B↓+NaCl
Sodium tetraphenylborate is as follows with the chemical equation of hydrocarbon ammonium salt:
The detection method flow chart of KCE content in a kind of activated water fracturing fluid that Fig. 1 provides for the embodiment of the present invention.
Referring to Fig. 1, in this activated water fracturing fluid, the detection method of KCE content includes:
Step 101, adds certain volume and excessive sodium tetraphenylborate standard solution, the potassium ion in precipitation activated water fracturing fluid in the activated water fracturing fluid of certain volume；
Step 102, then, adds corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, is titrated to corresponding color；
Step 103, quality according to the hydrocarbon ammonium salt in the hydrocarbon ammonium salt standard solution that titration uses, calculate the quality of the sodium tetraphenylborate reacted, obtain the quality of the sodium tetraphenylborate reacted with the potassium ion in activated water fracturing fluid, and then the ratio obtaining the of the fracturing fluid quality of activated water of the quality of potassium chloride in activated water fracturing fluid, the quality of this potassium chloride and described certain volume is the content of potassium chloride in this activated water fracturing fluid.
In a kind of activated water fracturing fluid that the embodiment of the present invention provides, the detection method of KCE content also includes:
After the activated water fracturing fluid of certain volume adds buffer, add excessive sodium tetraphenylborate standard solution；
In a kind of activated water fracturing fluid that the embodiment of the present invention provides in the detection method of KCE content, above-mentioned buffer is that Acetic acid-sodium acetate cushions night；Here, it is so that titrated solution keeps relatively low pH value that Acetic acid-sodium acetate cushions the effect at night, avoid raising with pH value in the remaining sodium tetraphenylborate standard solution process of hydrocarbon ammonium salt standard solution titration, cause that indicator is not reaching to titration end-point and variable color.Under the invention in the embodiment in face, Acetic acid-sodium acetate buffering night effect all identical, after no longer illustrate.
In this activated water fracturing fluid in the detection method of KCE content, acid-base indicator is bromophenol blue solution；With the sodium tetraphenylborate standard solution of hydrocarbon ammonium salt standard solution overtitration, being titrated to corresponding color is with the sodium tetraphenylborate standard solution of hydrocarbon ammonium salt standard solution overtitration, is titrated to blueness.Here, the metachromatic principle of bromophenol blue is when titration end-point, and bromophenol blue and excessive hydrocarbon ammonium salt generate a kind of coordination compound and show blueness.Under the invention in the embodiment in face, the metachromatic principle of bromophenol blue is all identical, after no longer illustrate.
In the above-described embodiment, also need to the quality of hydrocarbon ammonium salt in the hydrocarbon ammonium salt standard solution used according to titration, calculate the quality of the sodium tetraphenylborate reacted with hydrocarbon ammonium salt, add the step of calculating, thus invention further provides the detection method of KCE content in a kind of activated water fracturing fluid, it, by seeking the hydrocarbon ammonium salt standard solution titer to potassium chloride, is obtained the content of potassium chloride in activated water fracturing fluid, the following is the embodiment of the method.
The detection method flow chart of the content of potassium chloride in a kind of activated water fracturing fluid that Fig. 2 provides for further embodiment of this invention.
Referring to Fig. 2, in this activated water fracturing fluid, the detection method of the content of potassium chloride includes:
Step 201, potassium chloride standard solution V7Milliliter, adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；Add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V1Milliliter, after precipitating completely by potassium ion, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution is V1Milliliter；
Step 202, takes sodium tetraphenylborate standard solution X milliliter；Add described corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium normal saline solution that record titration uses is V0Milliliter；
Step 203, calculates the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；
Step 204, accurately pipettes the activated water fracturing fluid V milliliter filtered with dry filter paper, and being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Step 205, takes the activated water fracturing fluid V after dilution7Milliliter, adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；Add described corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V2Milliliter；In calculated activity water fracturing fluid, the content of potassium chloride is:Here, ρ is the of the fracturing fluid density of activated water of V milliliter, and unit is g/ml；
In this activated water fracturing fluid, the detection method of KCE content also includes:
At potassium chloride standard solution V7After milliliter, add buffer further, add excessive sodium tetraphenylborate solution X milliliter；
After taking sodium tetraphenylborate standard solution X milliliter, add buffer further, then with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；
Activated water fracturing fluid V after taking dilution7After milliliter, add buffer further, add excessive sodium tetraphenylborate solution X milliliter.
In this activated water fracturing fluid in the detection method of KCE content, described buffer is that Acetic acid-sodium acetate cushions night；
In this activated water fracturing fluid in the detection method of KCE content, described indicator is bromophenol blue solution；
Described hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, is titrated to corresponding color for hydrocarbon ammonium salt solution titration sodium tetraphenylborate solution, being titrated to blueness.
The described hydrocarbon ammonium salt remaining sodium tetraphenylborate solution of standard solution titration, being titrated to corresponding color is with the sodium tetraphenylborate solution of hydrocarbon ammonium salt solution overtitration, is titrated to blueness.
In an embodiment of the present invention, step 202 is blank assay, blank assay in order that the volume V of hydrocarbon ammonium salt that consumes when not having K+Precipitation of the sodium tetraphenylborate solution that obtains excessive X milliliter0.At the sodium tetraphenylborate standard solution used in test, potassium chloride standard solution and hydrocarbon ammonium salt standard solution, Acetic acid-sodium acetate buffer, when bromophenol blue solution is not changed in, blank assay is only done once.Namely, when the standardization of solution that test is used, this step can during sample test, be omitted.
In a upper embodiment, it it is the amount of the standard hydrocarbon ammonium salt asking remaining sodium tetraphenylborate standard solution to consume by direct method, operate relatively cumbersome, embodiment three is the amount of the standard hydrocarbon ammonium salt asking remaining sodium tetraphenylborate standard solution to consume with round-about way, this method is after being precipitated completely by the potassium ion in solution to be tested, precipitation is filtered out, the part only taking surplus solution is done experiment, calculate the amount of the hydrocarbon ammonium salt standard solution that sodium tetraphenylborate contained in a part of solution taken consumes, it is identical according to same substance ratio in this solution in same solution, calculate the amount of the hydrocarbon ammonium salt standard solution that remaining sodium tetraphenylborate standard solution consumes, this method calculates accurately, and it is easy and simple to handle relatively to go up a method, the following is the embodiment of the method.
In the activated water fracturing fluid that another embodiment of the present invention provides, the detection method of KCE content includes:
Potassium chloride standard solution V7After milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, then add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to described V4The subsequent filtrate of milliliter adds corresponding indicator, with the sodium tetraphenylborate standard solution in subsequent filtrate described in hydrocarbon ammonium salt standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V5Milliliter；According to formulaCalculate V1, here, V1After precipitating the potassium chloride standard solution potassium ion taken completely, the volume of the hydrocarbon ammonium salt standard solution used when remaining sodium tetraphenylborate reacts with hydrocarbon ammonium salt standard solution；In this embodiment of the invention, the V taken4The subsequent filtrate of milliliter is placed in the conical flask of 150 milliliters, V7=20, V3=100, X=25, V4=25。
Take sodium tetraphenylborate standard solution X milliliter；Add corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium normal saline solution that record titration uses is V0Milliliter；In this embodiment of the invention, this operation is also blank assay, effect with a upper embodiment empty test is identical, at the sodium tetraphenylborate standard solution used in test, potassium chloride standard solution and hydrocarbon ammonium salt standard solution, Acetic acid-sodium acetate buffer, when bromophenol blue solution is not changed in, blank assay is only done once.Namely, when the standardization of solution that test is used, this step can during sample test, be omitted.
Calculate the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；Calculate the density p of potassium chloride standard solution1=0.0008g/ml, m=ρ1V=0.0008g/ml × 20ml=0.016g.
Accurately pipetting the activated water fracturing fluid V milliliter filtered with dry filter paper, being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Take the activated water fracturing fluid V after dilution7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, then add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to described V4The subsequent filtrate of milliliter adds corresponding indicator, with the sodium tetraphenylborate standard solution in subsequent filtrate described in hydrocarbon ammonium salt standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V6Milliliter；According to formulaCalculate V2, V here2After precipitating the potassium ion in the activated water fracturing fluid taken completely, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution；
In calculated activity water fracturing fluid, the content of potassium chloride is:Here, ρ is the of the fracturing fluid density of activated water of described V milliliter.
In this activated water fracturing fluid, the detection method of KCE content also includes:
Potassium chloride standard solution V7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in after, add further Acetic acid-sodium acetate buffering night, then add excessive sodium tetraphenylborate standard solution X milliliter；In an embodiment of the present invention, affiliated Acetic acid-sodium acetate buffering night is 10 milliliters.
After taking sodium tetraphenylborate standard solution X milliliter, add Acetic acid-sodium acetate buffer further, then add corresponding indicator；In an embodiment of the present invention, affiliated Acetic acid-sodium acetate buffering night is 10 milliliters.
Take the activated water fracturing fluid V after dilution7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in after, add further Acetic acid-sodium acetate buffering night, then add excessive sodium tetraphenylborate standard solution X milliliter；In an embodiment of the present invention, affiliated Acetic acid-sodium acetate buffering night is 10 milliliters.In this embodiment of the invention, the indicator of addition is bromophenol blue solution, and the volume of the bromophenol blue solution of addition is 0.5 milliliter；It is titrated to corresponding color for being titrated to blueness.
In sum, technical scheme has the advantage that
1, the present invention adopts volumetric analysis to carry out the content of the potassium chloride in what mini-frac job site configured activated water fracturing fluid, and it is accurate that the method has result, easy and simple to handle, is not limited by instrument and equipment condition, it is possible to carry out the advantage used at the construction field (site).
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit protection scope of the present invention.All make within the spirit and principles in the present invention any amendment, equivalent replacement, improvement etc., be all contained in protection scope of the present invention.
Claims (2)
1. the detection method of KCE content in an activated water fracturing fluid, it is characterised in that described method includes:
Potassium chloride standard solution V7Milliliter adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation after adding buffer；Add corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V1Milliliter, after precipitating completely by potassium ion, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution is V1Milliliter；
After taking sodium tetraphenylborate standard solution X milliliter addition buffer, add described corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V0Milliliter；
Calculate the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；
Accurately pipetting the activated water fracturing fluid V milliliter filtered with dry filter paper, being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Take the activated water fracturing fluid V after dilution7Milliliter adds excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation after adding buffer；Add described corresponding indicator, with the hydrocarbon remaining sodium tetraphenylborate standard solution of ammonium salt standard solution titration, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V2Milliliter；In calculated activity water fracturing fluid, the content of potassium chloride is:Here ρ is the of the fracturing fluid density of activated water of described V milliliter；
Wherein, described buffer is that Acetic acid-sodium acetate cushions night；
Described indicator is bromophenol blue solution；
Described it is titrated to corresponding color for being titrated to blueness.
2. the detection method of KCE content in an activated water fracturing fluid, it is characterised in that described method includes:
Potassium chloride standard solution V7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, add after Acetic acid-sodium acetate buffer, add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to described V4The subsequent filtrate of milliliter adds corresponding indicator, with the sodium tetraphenylborate standard solution in subsequent filtrate described in hydrocarbon ammonium salt standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V5Milliliter；According to formulaCalculate V1, here, V1After precipitating the potassium chloride standard solution potassium ion taken completely, the volume of the hydrocarbon ammonium salt standard solution used when remaining sodium tetraphenylborate reacts with hydrocarbon ammonium salt standard solution；
After taking sodium tetraphenylborate standard solution X milliliter addition Acetic acid-sodium acetate buffer, add described corresponding indicator, with hydrocarbon ammonium salt standard solution titration sodium tetraphenylborate standard solution, be titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V0Milliliter；
Calculate the hydrocarbon ammonium salt standard solution titer to potassium chloride,Here m is by being taken V7The quality of the potassium chloride standard Chlorine in Solution potassium of milliliter；
Accurately pipetting the activated water fracturing fluid V milliliter filtered with dry filter paper, being placed in full scale line volume is V8In the volumetric flask of milliliter, it is diluted with water to the full scale line place of described volumetric flask；
Take the activated water fracturing fluid V after dilution7Milliliter, it is V that this solution is placed in full scale line volume3Volumetric flask in, add after Acetic acid-sodium acetate buffer, add excessive sodium tetraphenylborate standard solution X milliliter, complete K+Precipitation；After potassium ion precipitates completely, it is diluted with water to the full scale line of volumetric flask, filters the solution after dilution with dry filter paper, take subsequent filtrate V4Milliliter, then to described V4The subsequent filtrate of milliliter adds described corresponding indicator, with the sodium tetraphenylborate standard solution in subsequent filtrate described in hydrocarbon ammonium salt standard solution titration, is titrated to corresponding color；The volume of the hydrocarbon ammonium salt standard solution that record titration uses is V6Milliliter；According to formulaCalculate V2, V here2After precipitating the potassium ion in the activated water fracturing fluid taken completely, the volume of the hydrocarbon ammonium salt standard solution used when the remaining sodium tetraphenylborate in solution reacts with hydrocarbon ammonium salt standard solution；
In calculated activity water fracturing fluid, the content of potassium chloride is:Here ρ is the of the fracturing fluid density of activated water of described V milliliter；
Wherein, described indicator is bromophenol blue solution, described in be titrated to corresponding color for being titrated to blueness.
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