CN112946171A - Full-automatic EDTA titration detection method - Google Patents

Full-automatic EDTA titration detection method Download PDF

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Publication number
CN112946171A
CN112946171A CN202110059733.2A CN202110059733A CN112946171A CN 112946171 A CN112946171 A CN 112946171A CN 202110059733 A CN202110059733 A CN 202110059733A CN 112946171 A CN112946171 A CN 112946171A
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edta
solution
volumetric flask
sample
flask
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李富有
吴李靖
蒋海平
杨钢梁
单明军
刘永松
张军平
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Zhejiang Huaheng Traffic Construction Supervision Co ltd
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Zhejiang Huaheng Traffic Construction Supervision Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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
    • G01N21/79Photometric titration

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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  • General Physics & Mathematics (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to a full-automatic EDTA titration detection method, which comprises the following steps: 1) and stirring: weighing a stable material to be detected, putting the stable material into a sample bottle, and stirring the stable material by a spiral stirrer; 2) extracting turbid liquid of a sample to be detected: after stirring, starting an air pump to enable the suspension to enter a filter flask; 3) and adding various reagents and medicines: controlling a flow meter to respectively draw the solution from a calcium red indicator volumetric flask, a sodium hydroxide volumetric flask and an EDTA disodium volumetric flask into a filter flask by a solution suction display controller, and starting a magnetic stirrer to uniformly stir the mixed solution to be detected in the filter flask; 4) titration of the EDTA solution: and the solution sucking display controller controls the flow meter to draw the solution from the disodium EDTA volumetric flask, and the use amount of the disodium EDTA is read as the use amount of the EDTA of the sample when the sample is changed from rose red to pure blue. The invention has high detection precision and can quickly detect the dosage of cement or lime in the cement or lime stabilizing material.

Description

Full-automatic EDTA titration detection method
[ technical field ] A method for producing a semiconductor device
The invention relates to a method for quickly detecting the dosage of cement or lime, in particular to a full-automatic EDTA titration detection method, and belongs to the technical field of engineering material detection methods.
[ background of the invention ]
In the construction of composite stable soil roadbed and cement stabilized granular base course of highway and urban road, the key index for judging construction quality is the dosage of lime or cement. At present, EDTA titration method and direct-reading calcium meter method are mainly adopted for detection. However, both methods have certain defects in the actual detection process.
The EDTA titration method is operated by a tester by hands, so that the requirement on the skill and literacy of the tester is high, and the test precision is influenced by the stirring time, the stirring speed and the stirring mode of a sample. The accuracy of the standard reagent placement and storage conditions can affect the test results. The position at which the pipette sucks up the suspension influences the test results. The test result is influenced by the dosage of the calcium red indicator and the manual judgment of the titration end point. And the detection of a large batch of samples takes too long.
The lower limit of the standard dosage leaching liquor of the direct-reading calcium meter method is 6 percent, and the upper limit is 14, 16 or 18 percent. According to the current research results, the method is applied to roads of second grade and below, and urban secondary main road grades, the ash dosage of the composite stabilized soil base is only 5%, and the ash dosage can be met only by about 4% under the condition of adding other admixtures, so that the method adopting a direct-reading calcium meter method cannot meet the requirement of composite stabilized soil ash dosage detection of low ash dosage or adopting a secondary ash mixing process.
Therefore, in order to solve the above technical problems, it is necessary to provide an innovative full-automatic EDTA titration detection method to overcome the above-mentioned drawbacks in the prior art.
[ summary of the invention ]
In order to solve the problems, the invention aims to provide a full-automatic EDTA titration detection method which is simple in structure, convenient to use and high in detection precision and can be used for quickly detecting the dosage of cement or lime in a cement or lime stabilizing material.
In order to achieve the purpose, the invention adopts the technical scheme that: a full-automatic EDTA titration detection method adopts a full-automatic EDTA titration integrated detection device, and the detection device comprises the following detection steps:
1) and stirring:
weighing a stable material to be detected, putting the stable material into a sample bottle, and controlling a 10% ammonium chloride solution entering the sample bottle through a flowmeter; extending a paddle of a spiral stirrer into a sample bottle to realize full contact stirring of a sample to be detected and an ammonium chloride solution;
2) extracting turbid liquid of a sample to be detected:
after stirring is finished, the suspension does not need to be settled and placed, an air suction pump is started, the suspension is filtered by a sand core filter head, and the flow is controlled by a flowmeter, so that the quantity of the suspension to be detected entering a filter flask meets the requirement;
3) and adding various reagents and medicines:
controlling a flow meter to respectively pump a specified amount of solution from a calcium red indicator volumetric flask, a sodium hydroxide volumetric flask and an EDTA disodium volumetric flask into a filter flask by a solution sucking display controller, starting a magnetic stirrer to uniformly stir the solution to be detected mixed in the filter flask, wherein the sample is rosy;
4) titration of the EDTA solution:
the solution sucking display controller controls the flow meter to extract the solution from the EDTA disodium volumetric flask, the solution is quickly added firstly and then dripped in by inching, and the use amount of the EDTA disodium is read as the use amount of the EDTA of the sample when the sample is changed from rosy to pure blue.
The full-automatic EDTA titration detection method further comprises the following steps: the full-automatic EDTA titration integrated detection device comprises a base, a sample bottle, a spiral stirrer, a suction flask, a calcium red indicator volumetric flask, a sodium hydroxide volumetric flask, an EDTA disodium volumetric flask and a magnetic stirrer; the sample bottle, the filtration bottle, the calcium red indicator volumetric flask, the sodium hydroxide volumetric flask and the EDTA disodium volumetric flask are sequentially placed on the base; the spiral stirrer extends into the sample bottle; the sample bottle is connected with an ammonium chloride solution pipeline; the sample bottle, the calcium red indicator volumetric flask, the sodium hydroxide volumetric flask and the EDTA disodium volumetric flask are respectively connected to the filter flask through a connecting pipeline; the suction bottle is connected with a suction pump; the magnetic stirrer is arranged on the base, and the suction bottle is arranged on the magnetic stirrer.
The full-automatic EDTA titration detection method further comprises the following steps: the spiral stirrer is arranged on the base through a mounting bracket, is a lifting spiral stirrer, and comprises a paddle wing at the bottom, wherein the paddle wing is positioned in the sample bottle.
The full-automatic EDTA titration detection method further comprises the following steps: a flowmeter is respectively arranged on the ammonium chloride solution pipeline and each connecting pipeline; the flow meter on the ammonium chloride solution pipeline is positioned in the sample bottle; the flowmeter on the connecting pipeline is positioned in the filter flask.
The full-automatic EDTA titration detection method further comprises the following steps: a sand core filter head is arranged on a connecting pipeline for connecting the sample bottle and the filter flask; the sand core filter head is positioned in the sample bottle.
The full-automatic EDTA titration detection method further comprises the following steps: the base is provided with a stirring controller, a magnetic stirring switch and a plurality of solution sucking and displaying controllers; the stirring controller is electrically connected with and controls the spiral stirrer; the magnetic stirring switch is electrically connected with and controls the magnetic stirrer; the solution sucking display controller is electrically connected with the flow meter, and the flow meter is controlled to suck the solution from each volumetric flask.
The full-automatic EDTA titration detection method of the invention can also be as follows: in the step 4), the magnetic stirrer is kept started in the titration process, so that the mixed solution is always in a stirring state.
Compared with the prior art, the invention has the following beneficial effects: the full-automatic EDTA titration detection method provided by the invention is based on the EDTA titration principle, realizes automatic stirring, automatic solution extraction and reagent addition from the step of adding the composite stabilized soil or cement stabilized granular material sample, automatically records the consumption of EDTA, is controlled by a computer accurately, accurately reads the ETDA titration amount, and has the advantage of improving the detection efficiency. Standardized operation, reducing human errors and the like.
[ description of the drawings ]
FIG. 1 is a schematic diagram of the fully automatic EDTA titration integrated detection device of the present invention.
[ detailed description ] embodiments
Referring to the attached figure 1 of the specification, the invention relates to a full-automatic EDTA titration integrated detection device, which comprises a base 1, a sample bottle 2, a spiral stirrer 3, a suction filtration bottle 4, a calcium red indicator volumetric flask 5, a sodium hydroxide volumetric flask 6, a disodium EDTA volumetric flask 7, a magnetic stirrer 8 and the like.
Wherein, sample bottle 2, buchner flask 4, calcium red indicator volumetric flask 5, sodium hydroxide volumetric flask 6 and EDTA disodium volumetric flask 7 place in proper order on base 1. The sample vial 2 serves as a stirred vessel for the stabilized material to be tested. Various solutions can be added to and mixed in the filter flask 4 to achieve EDTA titration testing. The calcium red indicator volumetric flask 5 is used for storing a calcium red indicator solution. The sodium hydroxide volumetric flask 6 is used for storing 1.8% sodium hydroxide solution. The disodium EDTA volumetric flask 7 is used for storing disodium EDTA.
An ammonium chloride solution pipeline 21 is connected to the sample bottle 2, and a 10% ammonium chloride solution in an ammonium chloride volumetric flask 22 is added into the sample bottle 2 through the ammonium chloride solution pipeline 21.
The helical agitator 3 extends into the sample vial 2 and is mounted to the base 1 by a mounting bracket 31. In the present embodiment, the helical agitator 3 is a lifting helical agitator, the bottom of which includes a paddle 32, the paddle 32 is located in the sample bottle 2, and the paddle 32 rotates to mix and stir the ammonium chloride solution and the stabilizing material.
The sample bottle 2, the calcium red indicator volumetric flask 5, the sodium hydroxide volumetric flask 6 and the EDTA disodium volumetric flask 7 are respectively connected to the filter flask 4 through a connecting pipeline 9. The suction bottle 4 is connected with a suction pump 41, and negative pressure is generated in the suction bottle 4 through the suction pump 41, so that various solutions and mixed liquid of ammonium chloride and stable materials are sucked into the suction bottle 4.
Magnetic stirrers 8 install on base 1, and on magnetic stirrers 8 was arranged in to buchner flask 4, replaced the manual work through magnetic stirrers 8's magnetic stirring and rocked, can stir the interior liquid of buchner flask 4, made the reaction abundant.
And the ammonium chloride solution pipeline 21 and each connecting pipeline 9 are respectively provided with a flowmeter 10, and each flowmeter 10 can realize the control of the solution amount entering the filter flask 4 to accurately control the amount. Wherein the flow meter 10 on the ammonium chloride solution pipeline 21 is positioned in the sample bottle 2; the flow meter 10 on the connecting line 9 is located inside the filter flask 4. The solution is pumped and filtered into the filter flask 4 in sequence, when a certain solution reaches a set flow, the flowmeter 10 closes the corresponding connecting pipeline 9, and opens the subsequent connecting pipeline 9 to add other solutions.
A sand core filter head 22 is arranged on the connecting pipeline 9 connecting the sample bottle 2 and the filter flask 4. The sand core filter head 22 is positioned in the sample bottle 2, and the direct filtration of the mixed solution mixed by ammonium chloride and stable materials is realized, so that the standing clarification process of the mixed solution is replaced, and the efficiency and the artificial sampling error are improved.
Further, a stirring controller 11, a magnetic stirring switch 12 and a plurality of solution sucking display controllers 13 are arranged on the base 1. Wherein. Stirring controller 11 electric connection and control spiral agitator 3, its control that realizes stirring time and stirring rotational speed reduces the difference of manual stirring process and causes the result deviation, guarantees that stirring time, effect are all the same at every turn, and the stirring. The magnetic stirring switch 12 is electrically connected to and controls the magnetic stirrer 8, which realizes the shutdown of the magnetic stirring and the control of the stirring time. The solution sucking display controller 13 is electrically connected with the flow meter 10, and controls the flow meter 10 to extract the amount of the solution from each volumetric flask, so that the addition amount of each solution is accurately controlled.
The method for detecting the dosage of lime or cement in the stable material to be detected by adopting the full-automatic EDTA titration integrated detection device comprises the following steps:
1) and stirring:
weighing a stable material to be detected, putting the stable material into a sample bottle 2, and controlling a 10% ammonium chloride solution entering the sample bottle 2 through a flowmeter 10; the paddle 32 of the spiral stirrer 3 is extended into the sample bottle 2, so that the sample to be detected is fully contacted and stirred with the ammonium chloride solution;
2) extracting turbid liquid of a sample to be detected:
after stirring, the air pump 41 is started without waiting for the suspension to be precipitated and stand, the suspension is filtered by the sand core filter head 22, and the flow is controlled by the flowmeter 10, so that the amount of the suspension to be detected entering the filter flask 4 meets the requirement;
3) and adding various reagents and medicines:
the solution absorption display controller 13 controls the flowmeter 10 to respectively extract a specified amount of solution from the calcium red indicator volumetric flask 5, the sodium hydroxide volumetric flask 6 and the EDTA disodium volumetric flask 7 to enter the suction flask 4, and starts the magnetic stirrer 8 to uniformly stir the mixed solution to be detected in the suction flask 4, and at the moment, the sample is rosy red;
4) titration of the EDTA solution:
the solution sucking display controller 13 controls the flowmeter 10 to extract the solution from the disodium EDTA volumetric flask 7, the solution is quickly added firstly and then dripped in by inching, the use amount of the disodium EDTA as the use amount of the EDTA of the sample is read when the sample is changed from rose red to pure blue, and the magnetic stirrer 8 is kept started in the process, so that the mixed solution is always in a stirring state.
The full-automatic EDTA titration detection method can realize automatic addition of 10% ammonium chloride solution and automatic stirring; automatically filtering a mixed clarified liquid of a stable material sample and 10% ammonium chloride; automatically adding 1.8% sodium hydroxide solution and a calcium red indicator; realize the even replacement personnel of magnetic stirring automatically and rock, accurate control EDTA disodium titration volume to the realization contains from adding stable material to titrating EDTA use amount integration, and whole accurate control of computer reads ETDA titration volume accurately, improves detection efficiency. And (5) standardizing operation and reducing human errors.
Furthermore, the dosage of lime or cement in the mixture is determined by the EDTA consumption read by the full-automatic EDTA titration integrated detection device and a standard curve formulated by a laboratory theory.
The standard curve is established in the laboratory in advance, and the drawing test steps are as follows:
5 kinds of specimens were prepared, and about 300g of each specimen was taken for each of two kinds of specimens to prepare a test. The dosage of lime or cement for the 5 mixes should be: optimal dose, optimal dose ± 2% and + 4% ", two (wet mass) samples were taken for each dose, for a total of 10 samples. The moisture content of the soil sample should be equal to the optimal moisture content expected at the site, and the water added to the soil should be the same as that used at the site.
The average consumption (mL) of the same amount of the standard EDTA disodium salt as a stabilizing material was plotted on the ordinate and the amount (%) on the abscissa. The relationship between the two should be a smooth curve. Such as plain soil, cement or lime changes, the standard curve must be redone.
And determining the dosage of lime or cement in the mixture according to the consumption of the EDTA disodium standard solution read by the integrated equipment by using the drawn standard curve.
The above embodiments are merely preferred embodiments of the present disclosure, which are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present disclosure, should be included in the scope of the present disclosure.

Claims (7)

1. A full-automatic EDTA titration detection method is characterized in that: it adopts a full-automatic EDTA to titrate integrated detection device, and this detection device includes following detection step:
1) and stirring:
weighing a stable material to be detected, putting the stable material into a sample bottle, and controlling a 10% ammonium chloride solution entering the sample bottle through a flowmeter; extending a paddle wing of a spiral stirrer into a sample bottle to realize full contact stirring of a sample to be detected and an ammonium chloride solution;
2) extracting turbid liquid of a sample to be detected:
after stirring is finished, the suspension does not need to be settled and placed, an air suction pump is started, the suspension is filtered by a sand core filter head, and the flow is controlled by a flowmeter, so that the quantity of the suspension to be detected entering a filter flask meets the requirement;
3) and adding various reagents and medicines:
controlling a flow meter to respectively pump a specified amount of solution from a calcium red indicator volumetric flask, a sodium hydroxide volumetric flask and an EDTA disodium volumetric flask into a filter flask by a solution sucking display controller, starting a magnetic stirrer to uniformly stir the solution to be detected mixed in the filter flask, wherein the sample is rosy;
4) titration of the EDTA solution:
the solution sucking display controller controls the flow meter to extract the solution from the EDTA disodium volumetric flask, the solution is quickly added firstly and then dripped in by inching, and the use amount of the EDTA disodium is read as the use amount of the EDTA of the sample when the sample is changed from rosy to pure blue.
2. The fully automatic EDTA titration detection method according to claim 1, wherein: the full-automatic EDTA titration integrated detection device comprises a base, a sample bottle, a spiral stirrer, a suction flask, a calcium red indicator volumetric flask, a sodium hydroxide volumetric flask, an EDTA disodium volumetric flask and a magnetic stirrer; the sample bottle, the filtration bottle, the calcium red indicator volumetric flask, the sodium hydroxide volumetric flask and the EDTA disodium volumetric flask are sequentially placed on the base; the spiral stirrer extends into the sample bottle; the sample bottle is connected with an ammonium chloride solution pipeline; the sample bottle, the calcium red indicator volumetric flask, the sodium hydroxide volumetric flask and the EDTA disodium volumetric flask are respectively connected to the filter flask through a connecting pipeline; the suction bottle is connected with a suction pump; the magnetic stirrer is arranged on the base, and the suction bottle is arranged on the magnetic stirrer.
3. The fully automatic EDTA titration detection method according to claim 1, wherein: the spiral stirrer is arranged on the base through a mounting bracket, is a lifting spiral stirrer, and comprises a paddle wing at the bottom, wherein the paddle wing is positioned in the sample bottle.
4. The fully automatic EDTA titration detection method according to claim 2, characterized in that: a flowmeter is respectively arranged on the ammonium chloride solution pipeline and each connecting pipeline; the flow meter on the ammonium chloride solution pipeline is positioned in the sample bottle; the flowmeter on the connecting pipeline is positioned in the filter flask.
5. The fully automatic EDTA titration detection method according to claim 2, characterized in that: a sand core filter head is arranged on a connecting pipeline for connecting the sample bottle and the filter flask; the sand core filter head is positioned in the sample bottle.
6. The fully automatic EDTA titration detection method according to claim 2, characterized in that: the base is provided with a stirring controller, a magnetic stirring switch and a plurality of solution sucking and displaying controllers; the stirring controller is electrically connected with and controls the spiral stirrer; the magnetic stirring switch is electrically connected with and controls the magnetic stirrer; the solution sucking display controller is electrically connected with the flow meter, and the flow meter is controlled to suck the solution from each volumetric flask.
7. The fully automatic EDTA titration detection method according to claim 1, wherein: in the step 4), the magnetic stirrer is kept started in the titration process, so that the mixed solution is always in a stirring state.
CN202110059733.2A 2021-01-18 2021-01-18 Full-automatic EDTA titration detection method Pending CN112946171A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115980264A (en) * 2023-02-15 2023-04-18 陕西北元化工集团股份有限公司 Chemical component detection device in cement clinker

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GB1019892A (en) * 1961-05-11 1966-02-09 Courtaulds Ltd Automatic titration apparatus
US20090194430A1 (en) * 2008-01-31 2009-08-06 Eci Technology, Inc. Analysis of copper ion and complexing agent in copper plating baths
US20120252126A1 (en) * 2009-10-29 2012-10-04 Yulan Liang Method for analyzing and detecting calcium element in ore
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CN103616473A (en) * 2013-12-10 2014-03-05 武汉钢铁(集团)公司 Method for measuring iron content in direct reduction iron of steelmaking auxiliary material
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CN105388148A (en) * 2015-10-25 2016-03-09 镇江市丹徒区建筑工程质量检测中心 Method for determining lime dosage in lime stabilizing material
CN210166315U (en) * 2019-07-09 2020-03-20 中仪科立河北科技有限公司 Full-automatic COD analytical equipment
CN111351895A (en) * 2020-04-22 2020-06-30 汪洁 Automatic analysis device and automatic analysis method for measuring COD (chemical oxygen demand) in water

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Publication number Priority date Publication date Assignee Title
GB1019892A (en) * 1961-05-11 1966-02-09 Courtaulds Ltd Automatic titration apparatus
US20090194430A1 (en) * 2008-01-31 2009-08-06 Eci Technology, Inc. Analysis of copper ion and complexing agent in copper plating baths
US20120252126A1 (en) * 2009-10-29 2012-10-04 Yulan Liang Method for analyzing and detecting calcium element in ore
CN202962043U (en) * 2012-12-17 2013-06-05 山东商务职业学院 Filter device of potassium permanganate solution in detection of oil and foodstuffs
CN103616473A (en) * 2013-12-10 2014-03-05 武汉钢铁(集团)公司 Method for measuring iron content in direct reduction iron of steelmaking auxiliary material
CN103852466A (en) * 2014-02-21 2014-06-11 安费诺(天津)电子有限公司 Method for measuring chloride ion in acidity plating solution
CN105388148A (en) * 2015-10-25 2016-03-09 镇江市丹徒区建筑工程质量检测中心 Method for determining lime dosage in lime stabilizing material
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CN115980264A (en) * 2023-02-15 2023-04-18 陕西北元化工集团股份有限公司 Chemical component detection device in cement clinker

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Application publication date: 20210611