CN107727791A - The determination method of chlorion in a kind of quartz sand - Google Patents
The determination method of chlorion in a kind of quartz sand Download PDFInfo
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- CN107727791A CN107727791A CN201710965831.6A CN201710965831A CN107727791A CN 107727791 A CN107727791 A CN 107727791A CN 201710965831 A CN201710965831 A CN 201710965831A CN 107727791 A CN107727791 A CN 107727791A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/44—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte using electrolysis to generate a reagent, e.g. for titration
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Abstract
The invention discloses a kind of determination method of chlorion in quartz sand, its interpretation of result is：The content of chlorion is calculated as follows：In formula：W --- represent the content of chlorion, %；The concentration of C --- silver nitrate standard solution, mol/L；V1--- sample consumes the volume of silver nitrate standard solution, mL；M --- the sample size weighed, g；35.45 --- the molal weight of chlorion, g/mol.The method that the present invention determines chlorion using automatic potential titrator tests, method is easy, operation is rapid, can reduce labor intensity using this method, save analysis time.And the method investment of the invention is small, effect is good.A kind of the shortcomings that instant invention overcomes quartz sand chlorion without national standard method, and determination of chloride ion is comparatively laborious, analysis time is longer, there is provided relatively simple, quick analysis method.The chlorion gone out with water logging in quartz sand, in the presence of isopropanol stabilizer, the analysis of chlorion in quartz sand is carried out using automatical potentiometric titrimeter.
Description
Technical field
The present invention relates to a kind of detection method of chlorion, more particularly in a kind of quartz sand chlorion detection and analysis side
Method.
Background technology
Quartz sand is a kind of hard, wear-resisting, stable chemical performance silicate mineral, and its main mineral constituent is SiO2,
Quartz sand its chemistry, calorifics and mechanical performance have obvious anisotropy, and insoluble in acid, quartz has higher fire resistance.Work
Quartz sand is as solvent additive in industry copper metallurgy, it is ensured that smelting process SO2Reaction generation sodium sulfite generation is more stable, more holds
Easily separated silicate.Cl in quartz sand-Content is too high, can reduce the possibility of material surface passivating film formation, accelerate passivating film
Destroy, so as to promote local corrosion；Cl in corrosion processˉNot only richness is long-pending in point corrosion pit but also can not produce point corrosion pit
Rich product at region, this is probably process early stage that point corrosion pit is formed.Work as Cl-After concentration exceedes certain critical value, anode gold
Category will have been at the state of activation without being passivated.Therefore in Cl-Catalytic action under point corrosion pit can constantly expand, deepen.Its
Secondary Cl-There is catalytic action to crevice corrosion, iron loses electronics in anode when corrosion starts, with the continuous progress of reaction, iron
Constantly lose electronics, Fe in gap2+The substantial amounts of oxygen built up outside gap is not easily accessible, the strong Cl of migration-Enter gap
Interior and Fe2+Form high concentration, highly conductive FeCl2, FeCl2Hydrolysis produces H+, the pH value in gap is dropped to 3~4, so as to
Aggravation corrosion.Therefore the monitoring to chlorion is particularly important.
The analysis for chlorion in quartz sand detects at present, and the country does not have standard method of analysis, chloride test method
Substantially there are 4 kinds, mercury salt titration, silver nitrate turbidimetry method, the chromatography of ions, Chloride selective electrode method.And mercury salt titration, nitre
Acid silver-colored turbidimetry method operation is relatively complicated, also needs use toxic chemical reagent, and flow is longer, it is impossible to meets that production quickly divides
The needs of analysis.The domestic weight generally analyzed using the chromatography of ions and Chloride selective electrode method as chloride test at present
Means are wanted, wherein requirement of the chromatography of ions to sample is higher, therefore the quick measure of chlorion is always to perplex in quartz sand
Our production problem.
In order to solve the above problems, the present invention proposes a kind of new solution, develop in a kind of quartz sand chlorine from
The determination method of son.
The content of the invention
The problem of present invention aim to address chlorion in quartz sand without analysis method.
The present invention technical solution be：The process for preparation includes step：
The determination method of chlorion in a kind of quartz sand, the detection and analysis process include step：
Step 1：The instrument for testing and analyzing needs is chosen and is ready to, is used to work；
Step 2：Required detection and analysis reagent is made by concentration ratio；
Step 3：The reagent prepared is put into vessel according to a certain percentage and mixed；
Step 4：Mix reagent appropriate in vessel is taken out, is put into detecting instrument；
Step 5：Required sample is weighed out by a certain amount；
Step 6：The sample of taking-up is carried out dissolving heating and measure, step and control temperature are as follows：
50mL water cover upper surface ware is added in boiling 10min on electric hot plate, removes to be filtered with double-layer filter paper and is burnt in plastics
In cup, washing precipitation 3 times, 4mL isopropanol is added, with silver nitrate standard solution in being titrated on automatical potentiometric titrimeter
Terminal；
Step 7:Analyze testing result.
Preferably, the instrument that the detection and analysis need includes 855 type automatical potentiometric titrimeters and composite silver ring electrode.
Preferably, the formula of the reagent, it is by percentage：
Sodium chloride reference solution [C (NaCl)=0.0100mol/L]：By sodium chloride standard reagent in 500 DEG C~600 DEG C temperature
The lower calcination of degree weighs 0.5845 gram (claiming standard to 0.0002 gram), is placed in beaker, is dissolved with a small amount of water, by solution to constant weight
All it is transferred in 1000mL volumetric flasks, is diluted with water to scale, shakes up；
Silver nitrate standard solution：About 0.01mol/L：Prepare：Weigh 8.5 grams of silver nitrate (AgNO3) be dissolved in 5000mL water,
Shake up, solution is stored in brown bottle.
Preferably, the mix reagent is put into the detecting step and computational methods of detecting instrument：
20.00mL sodium chloride reference solution (2.2.3) is drawn, is placed in plastic cup, adds 40mL water, 4mL isopropanols, in
Demarcated on 855 automatical potentiometric titrimeters；
The concentration of silver nitrate standard solution is calculated as follows：
In formula：The concentration of C--- sodium chloride reference solutions, mol/L；
V1--- divide the volume for taking sodium chloride solution, mL；
V2--- the volume of consumption silver nitrate, mL.
Preferably, the digital independent of detecting instrument：
855 automatical potentiometric titrimeters, operating condition reference parameter are shown in Table 1；
The automatic potential titrator tests amount condition of table 1 855
Preferably, weigh quartz sand sample 0.5000g in 500mL beaker, add 50mL water cover upper surface ware in
10min to be boiled on electric hot plate, removes and is filtered with double-layer filter paper in plastic beaker, washing precipitates 3 times, adds 4mL isopropanol,
With silver nitrate standard solution in carrying out being titrated to terminal on automatical potentiometric titrimeter, automatical potentiometric titrimeter is beaten in advance before titration
Preheating half an hour is opened, under main operation interface, is first rinsed, flushing finishes to be titrated again.
Preferably, its interpretation of result is：
The content of chlorion is calculated as follows：
In formula：W --- represent the content of chlorion, %；
The concentration of C --- silver nitrate standard solution, mol/L；
V1--- sample consumes the volume of silver nitrate standard solution, mL；
M --- the sample size weighed, g；
35.45 --- the molal weight of chlorion, g/mol.
The beneficial effects of the invention are as follows：
(1) present invention determines the method for chlorion using automatic potential titrator tests, and method is easy, operation is rapid, uses this
Method can reduce labor intensity, save analysis time.And the method investment of the invention is small, effect is good.
(2) instant invention overcomes quartz sand chlorion without national standard method, determination of chloride ion is comparatively laborious, analysis time
A kind of the shortcomings that longer, there is provided relatively simple, quick analysis method.The chlorion gone out with water logging in quartz sand, in isopropyl
In the presence of alcohol stabilizer, the analysis of chlorion in quartz sand is carried out using automatical potentiometric titrimeter.
Embodiment
Embodiment 1
By following reagent concentration standard preparation reagents：
Sodium chloride reference solution [C (NaCl)=0.0100mol/L]：By sodium chloride standard reagent in 500 DEG C~600 DEG C temperature
The lower calcination of degree weighs 0.5845 gram (claiming standard to 0.0002 gram), is placed in beaker, is dissolved with a small amount of water, by solution to constant weight
All it is transferred in 1000mL volumetric flasks, is diluted with water to scale, shakes up；
Silver nitrate standard solution：About 0.01mol/L：Prepare：Weigh 8.5 grams of silver nitrate (AgNO3) be dissolved in 5000mL water,
Shake up, solution is stored in brown bottle.
Embodiment 2
It is measured as follows：
20.00mL sodium chloride reference solution (2.2.3) is drawn, is placed in plastic cup, adds 40mL water, 4mL isopropanols, in
Demarcated on 855 automatical potentiometric titrimeters；
The concentration of silver nitrate standard solution is calculated as follows：
In formula：The concentration of C--- sodium chloride reference solutions, mol/L；
V1--- divide the volume for taking sodium chloride solution, mL；
V2--- the volume of consumption silver nitrate, mL：
855 automatical potentiometric titrimeters, operating condition reference parameter are shown in Table 1；
The automatic potential titrator tests amount condition of table 1 855
Embodiment 3
Tested and analyzed as follows：
Quartz sand sample 0.5000g is weighed in 500mL beaker, adds 50mL water cover upper surface ware on electric hot plate
10min is boiled, removes and is filtered with double-layer filter paper in plastic beaker, washing precipitation 3 times, 4mL isopropanol is added, uses silver nitrate
Standard liquid opens automatical potentiometric titrimeter before titration preheating half in advance in carrying out being titrated to terminal on automatical potentiometric titrimeter
Hour, under main operation interface, first it is rinsed, flushing finishes to be titrated again.
The content of chlorion is calculated as follows：
In formula：W --- represent the content of chlorion, %；
The concentration of C --- silver nitrate standard solution, mol/L；
V1--- sample consumes the volume of silver nitrate standard solution, mL；
M --- the sample size weighed, g；
35.45 --- the molal weight of chlorion, g/mol.
In the use of the present invention, the reagent of analysis should reach the pure rank of analysis, analysis water distilled water or corresponding pure
The water of degree, the reagent used in demarcation should select benchmark to try.The water heating that 50.00mL is added by 0.5000g sample is boiled
Chlorion is leached, heating process wants cap surface ware, and heating boiling time ensures 10min.Filtered with double-deck Medium speed filter paper, mistake
Hot water injection's filter paper is used before filter, it is contemplated that the stability of determination of chloride ion, therefore 4mL isopropanols are added, it is molten with silver nitrate standard
Liquid on automatical potentiometric titrimeter in titrating to terminal.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any mark in claim should not be considered as to the involved claim of limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (7)
- A kind of 1. determination method of chlorion in quartz sand, it is characterised in that：The detection and analysis process includes step：Step 1：The instrument for testing and analyzing needs is chosen and is ready to, is used to work；Step 2：Required detection and analysis reagent is made by concentration ratio；Step 3：The reagent prepared is put into vessel according to a certain percentage and mixed；Step 4：Mix reagent appropriate in vessel is taken out, is put into detecting instrument；Step 5：Required sample is weighed out by a certain amount；Step 6：The sample of taking-up is carried out dissolving heating and measure, step and control temperature are as follows：50mL water cover upper surface ware is added in boiling 10min on electric hot plate, removes and is filtered with double-layer filter paper in plastic beaker, Washing precipitation 3 times, adds 4mL isopropanol, with silver nitrate standard solution in carrying out being titrated to terminal on automatical potentiometric titrimeter；Step 7:Analyze testing result.
- 2. the determination method of chlorion in a kind of quartz sand according to claim 1, it is characterised in that：The detection The instrument that analysis needs includes 855 type automatical potentiometric titrimeters and composite silver ring electrode.
- 3. the determination method of chlorion in a kind of quartz sand according to claim 1, it is characterised in that the reagent Formula, be by percentage：Sodium chloride reference solution [C (NaCl)=0.0100mol/L]：By sodium chloride standard reagent at a temperature of 500 DEG C~600 DEG C Calcination weighs 0.5845 gram (claiming standard to 0.0002 gram), is placed in beaker, is dissolved with a small amount of water, by solution whole to constant weight It is transferred in 1000mL volumetric flasks, is diluted with water to scale, shakes up；Silver nitrate standard solution：About 0.01mol/L：Prepare：Weigh 8.5 grams of silver nitrate (AgNO3) be dissolved in 5000mL water, shake up, Solution is stored in brown bottle.
- 4. the determination method of chlorion in a kind of quartz sand according to claim 1, it is characterised in that the mixing Reagent is put into the detecting step and computational methods of detecting instrument：20.00mL sodium chloride reference solution (2.2.3) is drawn, is placed in plastic cup, adds 40mL water, 4mL isopropanols, in 855 certainly Demarcated on electrokinetic potential titrator；The concentration of silver nitrate standard solution is calculated as follows：<mrow> <mi>C</mi> <mo>&lsqb;</mo> <msub> <mi>AgNO</mi> <mn>3</mn> </msub> <mo>&rsqb;</mo> <mo>=</mo> <mfrac> <mrow> <mi>C</mi> <mo>&times;</mo> <msub> <mi>V</mi> <mn>1</mn> </msub> </mrow> <msub> <mi>V</mi> <mn>2</mn> </msub> </mfrac> <mn>......</mn> <mrow> <mo>(</mo> <mn>1</mn> <mo>)</mo> </mrow> </mrow>In formula：The concentration of C--- sodium chloride reference solutions, mol/L；V1--- divide the volume for taking sodium chloride solution, mL；V2--- the volume of consumption silver nitrate, mL.
- 5. the determination method of chlorion in a kind of quartz sand according to claim 1 or 4, it is characterised in that detection The digital independent of instrument：855 automatical potentiometric titrimeters, operating condition reference parameter are shown in Table 1；The automatic potential titrator tests amount condition of table 1 855
- 6. the determination method of chlorion in a kind of quartz sand according to claim 1, it is characterised in that weigh quartz Sand sample product 0.5000g adds 50mL water cover upper surface ware in boiling 10min on electric hot plate, removes use in 500mL beaker Double-layer filter paper is filtered in plastic beaker, washing precipitation 3 times, 4mL isopropanol is added, with silver nitrate standard solution in automatic electric Carry out being titrated to terminal on the titrator of position, automatical potentiometric titrimeter is opened to preheating half an hour in advance, in main operation circle before titration Under face, first it is rinsed, flushing finishes to be titrated again.
- 7. the determination method of chlorion in a kind of quartz sand according to claim 1, it is characterised in that：Its result point Analyse and be：The content of chlorion is calculated as follows：<mrow> <mi>w</mi> <mrow> <mo>(</mo> <mi>%</mi> <mo>)</mo> </mrow> <mo>=</mo> <mfrac> <mrow> <mi>C</mi> <mo>&times;</mo> <msub> <mi>V</mi> <mn>1</mn> </msub> <mo>&times;</mo> <mn>35.45</mn> <mo>&times;</mo> <msup> <mn>10</mn> <mrow> <mo>-</mo> <mn>3</mn> </mrow> </msup> </mrow> <mi>m</mi> </mfrac> <mo>&times;</mo> <mn>100......</mn> <mrow> <mo>(</mo> <mn>2</mn> <mo>)</mo> </mrow> </mrow>In formula：W --- represent the content of chlorion, %；The concentration of C --- silver nitrate standard solution, mol/L；V1--- sample consumes the volume of silver nitrate standard solution, mL；M --- the sample size weighed, g；35.45 --- the molal weight of chlorion, g/mol.
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| CN110455983A (en) * | 2019-08-28 | 2019-11-15 | 福州大学 | The detection method of chloride ion content in a kind of determining sea sand |
| CN111735907A (en) * | 2020-08-04 | 2020-10-02 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
| CN113671111A (en) * | 2021-08-26 | 2021-11-19 | 金能科技股份有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
| CN114910531A (en) * | 2022-04-07 | 2022-08-16 | 浙江西热利华智能传感技术有限公司 | Chloride ion sensor-based concentration ratio online detection system and detection method |
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| US11940431B2 (en) * | 2019-08-28 | 2024-03-26 | Fuzhou University | Detection method for determining content of chlorine ions in marine sand |
| CN111735907A (en) * | 2020-08-04 | 2020-10-02 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
| CN111735907B (en) * | 2020-08-04 | 2020-12-08 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
| CN113671111A (en) * | 2021-08-26 | 2021-11-19 | 金能科技股份有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
| CN113671111B (en) * | 2021-08-26 | 2024-04-19 | 金能化学(齐河)有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
| CN114910531A (en) * | 2022-04-07 | 2022-08-16 | 浙江西热利华智能传感技术有限公司 | Chloride ion sensor-based concentration ratio online detection system and detection method |
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