CN107402208A - A kind of detection coupon and its detection method for examining mud acid - Google Patents
A kind of detection coupon and its detection method for examining mud acid Download PDFInfo
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- CN107402208A CN107402208A CN201710737656.5A CN201710737656A CN107402208A CN 107402208 A CN107402208 A CN 107402208A CN 201710737656 A CN201710737656 A CN 201710737656A CN 107402208 A CN107402208 A CN 107402208A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
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Abstract
The invention discloses a kind of detection coupon and its detection method for examining mud acid, the detection coupon is that one end open structure is closed in one end, is provided with sieve plate in the detection coupon, detection coupon is divided into the first detection layers and the second detection layers from bottom to top；First detection layers filling alizarin complexant, lanthanum nitrate and the silica gel；The second detection layers filling sodium carbonate and silica gel.If the first detection layers are blue red secondary colour, and the second detection layers have gas and with white opacity, then testing liquid is mud acid；If the first detection layers occur to be red without blueness, and the second detection layers only have gas but do not occur white opacity, then testing liquid is hydrochloric acid.The detection coupon of the present invention can intuitively distinguish mud acid, hydrochloric acid and water very much, and the inspection detection coupon after does not pollute the environment, and has stronger promotion and use value.
Description
【Technical field】
The present invention relates to one kind to detect coupon, more particularly to a kind of detection coupon and its detection method for examining mud acid, uses
Sour chemical composition is used in oilfield development process in detecting.
【Background technology】
Oil field can carry out pressure break and acidizing treatment on stream, to improve development effectiveness.Hydrochloric acid and mud acid are all oil
Field often with acid stimulation agent, can effectively release shaft bottom and nearby block, increase well yield.Due to hydrochloric acid and mud acid property class
Seemingly, it is difficult to distinguish if without visible marking.If false touch mud acid can cause high risks to the person, because containing a large amount of hydrogen in mud acid liquid
Fluoric acid, fluorine ion therein has strong dehydration and corrosiveness to tissue, and fluorine is one of most active nonmetalloid, energy
With hydrogen ion strong bonded.After skin and hydrofluoric acid contact, acid solution constantly dissociation penetrates into deep tissues, dissolves cell membrane, meeting
Make epidermis, corium, hypodermis and to muscle layer liquefaction and necrosis.Fluorine ion combines to form slightly solubility with the calcium in tissue and magnesium ion
Salt, the reduction of calcium ion cause cell to face the increase of potassium ion permeability, and potassium ion to extracellular from causing nerve into the cell
The depolarising of cell and cause severe pain.
To avoid that false touch accident occurs at acidification of oil field scene, the general method for detecting mud acid is spot sampling, interior point
Analysis, its strongly professional, complex procedures, time and financial resources are expended, it is ageing not strong.Using GB/T 5009.18---2003 expansion
The electronic detector that the principles such as scattered-fluorine reagent colorimetric method make, operating method is complicated, high to personnel qualifications, the scope of application
Limitation, instrument are heavy, and the reagent after is not allowed disposable, so as to be polluted to environment, is not suitable in acidification of oil field
Applied under the particular surroundings such as scene.
Therefore, present invention is generally directed to the problems of the prior art, there is provided a kind of detection coupon for examining mud acid is so as to fast
Speed easily detects, distinguishes hydrochloric acid and mud acid, avoids false touch mud acid from damaging people, and the reagent after is made to environment
Into pollution.
【The content of the invention】
The invention provides a kind of detection coupon and its detection method for examining mud acid, passes through the detection of observation first, second
The differential responses phenomenon of layer, makes a distinction to mud acid and hydrochloric acid.
The present invention uses following technical scheme：
A kind of detection coupon for examining mud acid, the detection coupon include passing through color detection fluorine ion successively from sampling end
The first detection layers, determine by liquid phase-state change the second detection layers of fluorine ion, and reaction intermediates matter is carried out
3rd detection layers of sum；The mixture of the first detection layers filling alizarin complexant, lanthanum nitrate and silica gel；Described second
Detection layers fill the mixture of sodium carbonate and silica gel, mixture of the 3rd detection layers filled with alkali and silica gel.
The sampling layer and the first detection layers, the first detection layers and the second detection layers, the second detection layers and the 3rd detection layers
Between separated by sieve plate.
Silica gel is filled with the sampling layer.
The silica gel is silica gel particle.
The detection coupon is placed in protective case.
The protective case includes lower protective case and upper protective case, the protective case offer for observe the first detection layers and
The observation window of second detection layers color change.
A kind of detection method for detecting coupon for examining mud acid, detection coupon is put into testing liquid, if the first detection
Layer is blue red mixture, and the second detection layers have gas and with white opacity, then testing liquid is mud acid；If the first detection layers
Occur for red without blueness, and the second detection layers only have gas but do not occur white opacity, then testing liquid is hydrochloric acid.
After detecting coupon and being put into testing liquid, according to diffusion-fluorine reagent colorimetric method principle, hydrofluoric acid, lanthanum nitrate and
Alizarin complexant generates blue ternary complexes, and hydrochloric acid, lanthanum nitrate and alizarin complexant generate red ternary complexing
Thing.
If testing liquid is mud acid, the complete hydrofluoric acid of silica gel particle and the first detection layers unreacted in the second detection layers
Silicon tetrafluoride gas is further generated, the gas generates white opacity after being absorbed by sodium carbonate and releases colourless gas.
The sour gas and excess acid of first detection layers and the second detection layers are neutralized by the alkali of the 3rd detection layers.
Compared with prior art, the present invention at least has the advantages that：
Present invention detection coupon is disposed with the first detection layers, the second detection layers and the 3rd detection layers in sampling end.Such as
Fruit testing liquid is mud acid, then the first detection layers are red blue secondary colour, and the second detection layers have gas to produce and with white muddy
It is turbid；And if testing liquid is hydrochloric acid, then the first detection layers occur to be red and without blueness, and the second detection layers only have gas but
Do not occur white opacity；It is water or akaline liquid that liquid is detected if the first detection layers and the second detection layers are unchanged.In this way, this
Invention detection coupon can identify mud acid and hydrochloric acid easily according to color.Detection speed is fast, testing result is accurate, and detects coupon
Simple in construction, easy to operate, cost is cheap, can carry with, and is especially advantageous for popularizing on oil field.
Further by the sour gas and excess acid in the highly basic of the 3rd detection layers with the first two detection layers, tried in detection
Detection is gathered in rod and liquid waste processing is integrated, it is dirty to caused by environment to avoid the chemical substance detected after use in coupon
Dye.
【Brief description of the drawings】
Fig. 1 is the schematic diagram of present invention detection coupon；
Fig. 2 is present invention detection coupon protective case entirety front view；
Fig. 3 is that present invention detection coupon protects upper jacket front view；
Fig. 4 is protective case front view under present invention detection coupon；
Fig. 5 is present invention detection coupon protective case top view.
Wherein：1st, the first detection layers；2nd, the second detection layers；3rd, the 3rd detection layers；4th, layer is sampled；5th, sieve plate；6th, detection examination
Rod；7th, protective case；8th, upper protective case；9th, lower protective case；10th, observation window.
【Embodiment】
The invention provides a kind of detection coupon for examining mud acid, by observing the differential responses of two layers of detection layers, to soil
Acid and hydrochloric acid are made a distinction, and sour gas caused by excess acid and reaction neutralize by third layer and reclaims innoxious place
Reason.
Referring to Fig. 1, a kind of detection coupon for examining mud acid, material is clear glass or clear PE, preferably clear PE.Inspection
Prod is the cylinder hollow pipe of one end open one end closing, is set in detection coupon and is arranged at intervals 3 sieve plates 5, and sieve plate 5 will
Detection coupon is divided into sampling layer 4, the first detection layers 1, the second detection layers 2 and the 3rd detection layers 3 successively from bottom to top, samples layer
4 be opening conical structure, and it is filled with silica gel particle.Wherein the first detection layers 1, the second detection layers 2 and the 3rd detection layers 3
Volume ratio is 3:2:3.
Alizarin complexant, lanthanum nitrate, sodium acetate and silica gel particle, wherein alizarin ammonia carboxylic are filled in first detection layers 1
Complexing agent, lanthanum nitrate, sodium acetate proportioning are 1:(1.2~1.5):(500~1000).
Sodium carbonate and silica gel particle are filled in second detection layers 2.
Sodium hydroxide and silica gel particle are filled in 3rd detection layers 3.
Because silica gel particle has strong absorptive, draw detection liquid as carrier and be transferred to each detection layers.
Fig. 2-5 are referred to, detection coupon is placed on made of opaque PP in protective case 7, and protective case 7 includes upper protective case
8 and lower protective case 9, upper protective case 8 is sleeved on the detection layers for examining mud acid detection coupon, and lower protective case is sleeved on detection coupon
Layer 4 is sampled, offers observation window 10 in corresponding first detection layers 1 of upper protective case and the position of the second detection layers 2, observation color becomes
Change.
(explanation is described in detail to reaction mechanism of the detection coupon respectively with mud acid, hydrochloric acid or water below：It is same in mud acid
When include hydrochloric acid and hydrofluoric acid).
A, liquid to be detected is if mud acid.
Sample layer：Due to containing hydrofluoric acid in mud acid, therefore hydrofluoric acid reacts with silica gel.
4HF+H2SiO3=SiF4↑+3H2O
First detection layers：If determinand is mud acid, according to GB/T 5009.18---2003 diffusion-fluorine reagent colorimetric
Method principle, hydrofluoric acid, lanthanum nitrate and alizarin complexant generate blue ternary complexes in pH 5.0, and complex compound color is with fluorine
Ion concentration increases and deepened；Simultaneously as the presence of hydrofluoric acid, hydrofluoric acid further react with silica gel：
4HF+H2SiO3=SiF4↑+3H2O
Hydrochloric acid, lanthanum nitrate, alizarin complexant generate red ternary complexes in pH about 4.3；Wherein the first detection layers
In sodium acetate be used for adjust pH value and reaction rate.
Therefore, if determinand is mud acid, it is red blue secondary colour that the first detection layers, which show color,.What the first detection layers were related to
Reaction is as follows：
4HF+H2SiO3=SiF4↑+3H2O
Second detection layers：Sampling layer and the silicon tetrafluoride gas of the first detection layers generation enter the second detection through sieve plate
Layer, because the second detection layers are filled with sodium carbonate, therefore, silicon tetrafluoride gas is absorbed by sodium carbonate, meanwhile, in the second detection layers
Silica gel particle do not reacted completely with the first detection layers 1 further hydrofluoric acid reaction generate silicon tetrafluoride gas again, should
Gas is absorbed by sodium carbonate in the lump, generates white opacity and releases colourless gas (minute bubbles).First detection layers are without completely anti-
The hydrochloric acid answered further reacts with sodium carbonate, generates carbon dioxide.
The reaction that second detection layers are related to is as follows：
4HF+H2SiO3=SiF4↑+3H2O
3SiF4+2Na2CO3+2H2O=H4SiO4↓+2Na2SiF6↓+2CO2
Chemically reacted if this layer of excessive acid as follows：
Na2CO3+ 2HCl=2NaCl+H2O+CO2↑
If this layer of acid on a small quantity if chemical reaction it is as follows：
Na2CO3+ HCl=NaCl+NaHCO3
3rd detection layers：Using the strong basicity of sodium hydroxide neutralize the first detection layers and the second detection layers sour gas and
Excess acid.
4HF+H2SiO3=SiF4↑+3H2O
Chemical reaction is as follows if this layer of carbon dioxide is excessive：
NaOH+CO2=NaHCO3
If this layer of carbon dioxide on a small quantity if chemical reaction it is as follows：
2NaOH+CO2=Na2CO3+H2O and H++OH-=H2O
B, liquid to be detected is as follows if hydrochloric acid, detection coupon chemical reaction：
Sample layer：Due to not containing hydrofluoric acid, and hydrochloric acid does not react with silica gel, and therefore, any reaction does not occur for the layer.
First detection layers：(about 4.3) generation under appropriate pH of hydrochloric acid, lanthanum (III), fluorine reagent (alizarin complexant) is red
Color ternary complexes；Wherein the sodium acetate of the first detection layers is used to adjust pH value and reaction rate.
Second detection layers：Na2CO3+ 2HCl=2NaCl+H2O+CO2↑
3rd detection layers：2NaOH+CO2=Na2CO3+H2O
H++OH-=H2O
C, liquid to be detected is not reacted if water or alkali, detection each detection layers of coupon.
, tentatively can be with if the first detection layers display color is blue red secondary colour from the above, it can be seen that in detection
The determinand is judged for mud acid, if the first detection layers display color is red, without blueness, then preliminary judgement determinand
For hydrochloric acid；If the second detection layers are shown and gas generates and white opacity occurs, and the primitive decision determinand is mud acid, such as
The detection layers of fruit second only have gas but do not occur white opacity, then the primitive decision determinand is hydrochloric acid.
Elaborated below for embodiment：
Embodiment 1
A kind of detection coupon for examining mud acid, detection coupon are the cylinder hollow pipe of one end open one end closing, are being detected
Set in coupon and be arranged at intervals 3 sieve plates 5, detection coupon is divided into sampling layer 4, the first detection layers 1, the successively from bottom to top
Two detection layers 2 and the 3rd detection layers 3, sampling layer 4 are opening cone.Wherein the first detection layers 1, the second detection layers 2 and the 3rd
The volume ratio of detection layers 3 is 3:2:3.
Sample the filling gel particle of layer 4；First detection layers 1 filling alizarin complexant, lanthanum nitrate, sodium acetate and silica gel
Particle, wherein alizarin complexant, lanthanum nitrate, sodium acetate proportioning are 1:1.2:500；Second detection layers 2 fill sodium carbonate and
Silica gel particle；3rd detection layers 3 fill sodium hydroxide and silica gel particle.
Embodiment 2
A kind of detection coupon for examining mud acid, detection coupon are the cylinder hollow pipe of one end open one end closing, are being detected
Set in coupon and be arranged at intervals 3 sieve plates 5, detection coupon is divided into sampling layer 4, the first detection layers 1, the successively from bottom to top
Two detection layers 2 and the 3rd detection layers 3, sampling layer 4 are opening cone.Wherein the first detection layers 1, the second detection layers 2 and the 3rd
The volume ratio of detection layers 3 is 3:2:3.
Sample the filling gel particle of layer 4；First detection layers 1 filling alizarin complexant, lanthanum nitrate, sodium acetate and silica gel
Particle, wherein alizarin complexant, lanthanum nitrate, sodium acetate proportioning are 1:1.5:1000.；Second detection layers 2 fill sodium carbonate
And silica gel particle；3rd detection layers 3 fill calcium hydroxide and silica gel.
Embodiment 3
A kind of detection coupon for examining mud acid, detection coupon are the cylinder hollow pipe of one end open one end closing, are being detected
Set in coupon and be arranged at intervals 3 sieve plates 5, detection coupon is divided into sampling layer 4, the first detection layers 1, the successively from bottom to top
Two detection layers 2 and the 3rd detection layers 3, sampling layer 4 are opening cone.Wherein the first detection layers 1, the second detection layers 2 and the 3rd
The volume ratio of detection layers 3 is 3:2:3.
Sample the filling gel particle of layer 4；First detection layers 1 filling alizarin complexant, lanthanum nitrate, sodium acetate and silica gel
Particle, wherein alizarin complexant, lanthanum nitrate, sodium acetate proportioning are 1:1.35:800.；Second detection layers 2 fill sodium carbonate
And silica gel particle；3rd detection layers 3 fill potassium hydroxide and silica gel.
The present invention examines the preparation method of the detection coupon of mud acid to comprise the following steps：
1st, silica gel particle loads the detection orlop of coupon 6, forms sampling layer 4, is then charged into sieve plate 5；
2nd, alizarin complexant, lanthanum nitrate, sodium acetate are according to 1:(1.2~1.5):(500~1000) prepare, Ran Houjia
Enter silica gel particle stirring filling and form the first detection layers 1 to step 1 sieve plate 5, be then again loaded into sieve plate 5；
3rd, the second detection layers 2, Ran Houzai are formed on filling to step 2 sieve plate 5 after sodium carbonate and silica gel particle are sufficiently mixed
Secondary loading sieve plate 5；
4th, the 3rd detection layers 3 are formed after sodium hydroxide and silica gel particle are sufficiently mixed on filling to step 3 sieve plate；
5th, after the completion of filling, by detection coupon charging port sealing.
6th, step 5 is detected into coupon and loads protection overcoat 7.
The present invention examines mud acid detection coupon to be stored at shady and cool dry.
The present invention examines mud acid detection coupon application method as follows：
Lower protective case 9 is first turned on, is then put into sampling layer 4 in acid to be measured three to five seconds.Take out detection detection coupon
And lower protective case 9 is covered, the change of the first detection layers and the second detection layers is observed by observation window 10.
If A, the first detection layers color is red blue secondary colour, the second detection layers have bubble formation and white opacity occur, then
Detection liquid is mud acid.
If B, the first detection layers are red, the second detection layers have gas generation, then it is hydrochloric acid to detect liquid.
C, if without phenomenon, detection liquid is water or akaline liquid for the first detection layers and the second detection layers.
The present invention examines the detection coupon of mud acid is simple to operate can quickly distinguish hydrochloric acid, mud acid and water, and its make it is simple,
Cost is low, has stronger promotion and use value.
Claims (10)
- A kind of 1. detection coupon for examining mud acid, it is characterised in that：The detection coupon (6) includes passing through face successively from sampling end The first detection layers (1) of color detection fluorine ion, the second detection layers (2) for determining by liquid phase-state change fluorine ion, and it is right The 3rd detection layers (3) that reaction intermediates matter is neutralized；First detection layers (1) the filling alizarin complexant, nitric acid The mixture of lanthanum and silica gel；The mixture of second detection layers (2) the filling sodium carbonate and silica gel, the 3rd detection layers filling There is the mixture of alkali and silica gel.
- A kind of 2. detection coupon for examining mud acid according to claim 1, it is characterised in that：The sampling layer (4) and the Pass through between one detection layers (1), the first detection layers (1) and the second detection layers (2), the second detection layers (2) and the 3rd detection layers (3) Sieve plate (5) separates.
- A kind of 3. detection coupon for examining mud acid according to claim 1, it is characterised in that：It is filled with the sampling layer Silica gel.
- A kind of 4. detection coupon for examining mud acid according to any one of claim 1 to 3, it is characterised in that：The silicon Glue is silica gel particle.
- A kind of 5. detection coupon of inspection mud acid according to any one of claim 1-3, it is characterised in that：The detection Coupon (6) is placed in protective case (7), and protective case (7) is offered for observing the first detection layers (1) and the second detection layers (2) The observation window (10) of color change.
- A kind of 6. detection coupon for examining mud acid according to claim 5, it is characterised in that：The protective case (7) includes Lower protective case (9) and upper protective case (8).
- A kind of 7. detection method based on the detection coupon that mud acid is examined described in claim 1, it is characterised in that：Coupon will be detected It is put into testing liquid, if the first detection layers are blue red secondary colour, and the second detection layers have gas and with white opacity, then treat Survey liquid is mud acid；If the first detection layers occur to be red without blueness, and the second detection layers only have gas but not occurred white muddy Turbid, then testing liquid is hydrochloric acid, and it is water or akaline liquid to detect liquid if the first detection layers and the second detection layers are unchanged.
- A kind of 8. detection method for detecting coupon for examining mud acid according to claim 7, it is characterised in that：When detection tries After rod is put into testing liquid, according to diffusion-fluorine reagent colorimetric method principle, hydrofluoric acid, lanthanum nitrate and alizarin complexant life Au bleu ternary complexes, hydrochloric acid, lanthanum nitrate and alizarin complexant generate red ternary complexes.
- A kind of 9. detection method for detecting coupon for examining mud acid according to claim 7, it is characterised in that：If prepare liquid Body is mud acid, then the silica gel particle in the second detection layers and the complete hydrofluoric acid of the first detection layers unreacted further generate tetrafluoride Silicon gas, the gas generate white opacity after being absorbed by sodium carbonate and release colourless gas.
- A kind of 10. detection method for detecting coupon for examining mud acid according to claim 7, it is characterised in that：First inspection The sour gas and excess acid for surveying layer and the second detection layers are neutralized by the alkali of the 3rd detection layers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710737656.5A CN107402208B (en) | 2017-08-24 | 2017-08-24 | Detection test bar for detecting earthic acid and detection method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710737656.5A CN107402208B (en) | 2017-08-24 | 2017-08-24 | Detection test bar for detecting earthic acid and detection method thereof |
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| CN107402208B CN107402208B (en) | 2023-09-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111965180A (en) * | 2020-08-28 | 2020-11-20 | 中国石油化工股份有限公司 | Quantitative detection method for alkyl nitrate in diesel oil |
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