CN109187530A - Zinc, aluminum content tests method in a kind of industry ZnSO4 - Google Patents
Zinc, aluminum content tests method in a kind of industry ZnSO4 Download PDFInfo
- Publication number
- CN109187530A CN109187530A CN201811345326.2A CN201811345326A CN109187530A CN 109187530 A CN109187530 A CN 109187530A CN 201811345326 A CN201811345326 A CN 201811345326A CN 109187530 A CN109187530 A CN 109187530A
- Authority
- CN
- China
- Prior art keywords
- zinc
- edta
- added
- solution
- aluminium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Abstract
The invention discloses zinc, aluminum content tests method in a kind of industry ZnSO4, comprising the following steps: prepares sample solution；Excessive EDTA standard solution is added into gained sample solution, mixes, is cooled to room temperature after heating, carries out complex reaction, obtains mixed solution；With the excessive ETDA titer of Zinc standard solution back titration, buffer is added and adjusts pH, using xylenol orange as indicator, with the ETDA of Zinc standard solution overtitration；Ammonium fluoride is added, destroys the complexing of aluminium and EDTA, the EDTA with aluminium complexing is precipitated；The EDTA being precipitated again with Zinc standard solution titration, to measure the content of zinc and aluminium.Detection method of the invention has highly sensitive, accuracy and stability, easy to operate, analysis speed is fast.
Description
Technical field
The present invention relates to a kind of chemical industry measurement method, in particular to zinc, aluminum content tests side in a kind of industry ZnSO4
Method.
Background technique
In the process of manufacture of industrial ZnSO4, due to mineral resources, pipeline, equipment, raw material etc. in its preparation process
The reason of, a large amount of Al is contained usually in the ZnSO4 prepared3+, decline the percentage composition of zinc in product.Traditional
The measuring method of Zn content is to directly adopt EDTA complexometric titration in industrial ZnSO4, but due to EDTA and Zn2+And Al3+
The stability constant of complex compound is very close, and the Zn content finally measured is really Zn2+And Al3+The sum of, it can not be by zinc and aluminium
Content determines respectively to be come, and aluminium disturbs Direct spectrophotometry as a result, leading to Zn in continuous mode2+The accuracy of content analysis result
It is poor with precision.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the deficiencies of the prior art and provide a kind of easy to operate, accuracy
Height, precision are good, analyze zinc, aluminum content tests method in fireballing industry ZnSO4 solution.
The technical solution adopted by the present invention to solve the technical problems is: zinc, aluminum content tests in a kind of industry ZnSO4
Method, comprising the following steps:
1) sample solution is prepared；
2) excessive EDTA standard solution is added into sample solution obtained by step 1), mixes, is cooled to room temperature after heating, carry out
Complex reaction obtains mixed solution；
3) the excessive ETDA titer of Zinc standard solution back titration is used, buffer is added and adjusts pH, using xylenol orange as indicator,
With the ETDA of Zinc standard solution overtitration；
4) ammonium fluoride is added, destroys the complexing of aluminium and EDTA, the EDTA with aluminium complexing is precipitated；
5) EDTA being precipitated again with Zinc standard solution titration, to measure the content of zinc and aluminium.
Zinc and aluminium are first complexed using excessive EDTA, form EDTA- zinc complex and EDTA- aluminium complex, then with zinc mark
Uncomplexed EDTA in quasi- solution titration solution, to learn the total amount of the EDTA with zinc and aluminium complexing.Due to ammonium fluoride and aluminium
Complex compound stability constant ratio EDTA and aluminium complex compound constant it is big, then the aluminium in EDTA- aluminium is complexed out with ammonium fluoride
Come, so that the EDTA with aluminium complexing be precipitated, then titrate the EDTA of the EDTA(separated out and aluminium complexing with Zinc standard solution), then may be used
The dosage for knowing the EDTA of EDTA and aluminium complexing, directly determines the content of aluminium, is subtracted by the total amount that EDTA is complexed with zinc and aluminium
The dosage of EDTA and the EDTA of aluminium complexing learn the dosage of EDTA and zinc complexing, the indirect determination content of zinc.
Further, described the step of preparing sample solution are as follows: weigh sample to be tested 1g, the dense salt of 30-35% is added in the sample
Acid 2~20ml, 60-70% 2~15ml of concentrated nitric acid, heating steam to wet salt, remove cooled to room temperature, sample plus water are stirred
It mixes and is diluted to 1000ml sample solution is made.
It will form white crystals since zinc sulfate is directly dissolved in water, need to control the pH of lysate within 6-7.5,
Otherwise zinc sulfate can not completely dissolve in water, and therefore, concentrated hydrochloric acid and concentrated nitric acid, which is added, makes solution in after acid, can just make sulphur
Sour zinc completely dissolves in water.
Further, EDTA standard solution is added in the step 2, after being boiled with soft fire 2min, is cooled to room with flowing water immediately
Temperature.
Further, the concentration of the EDTA standard solution is 0.015mol/L.
Further, the buffer is HAc-NaAc buffer, and the volume of the buffer is 20-40mL, and the pH is
5-6, the concentration of the Zinc standard solution are 0.1mg/mL.
Further, in the step 4, mass fraction 30-40% ammonium fluoride is added, shakes up, stand 5-10min, and heat
To 30 DEG C~40 DEG C, fluorine ion is complexed completely with tin ion.
Zinc in a kind of industry ZnSO4 of the present invention, aluminum content tests method the utility model has the advantages that the present invention by by EDTA network
Reaction and the combination of back titration method are closed, first zinc and aluminium is complexed with EDTA, then use Zinc standard solution back titration EDTA, is directly surveyed
Aluminium content, thus the indirect determination content of zinc, this method avoid the interference of aluminium during zinc-content determination, simultaneously will
The content of aluminium, which also determines, to be come, and improves the accuracy of zinc-content determination, and various reagents according to the present invention are common
Chemical reagent, the content of aluminum and zinc can be measured simultaneously by not needing special analysis instrument, and process is simple, measurement the period it is short, at
This is lower, easy to promote and utilize.
Specific embodiment
The invention will be further described with reference to embodiments, but these specific embodiments do not limit in any way
Protection scope of the present invention.
Embodiment 1
Zinc, aluminum content tests method in a kind of industry ZnSO4, comprising the following steps:
1) sample to be tested 1g is weighed, 30% concentrated hydrochloric acid 10ml, 60% concentrated nitric acid 15ml is added in the sample, heating is steamed to wet salt,
Cooled to room temperature is removed, sample is added water and stirred and is diluted to 1000ml, prepares sample solution；
2) 40mL 0.015mol/L EDTA standard solution is added into sample solution obtained by step 1), mixes, heating, small fire
It after boiling 2min, is cooled to room temperature with flowing water, carries out complex reaction, obtain mixed solution；
3) the excessive ETDA titer of Zinc standard solution back titration of 0.1mg/mL is used, addition mass fraction is 30%HAc-NaAc
It is 5 that buffer, which adjusts pH, using xylenol orange as indicator, xylenol orange indicator 3~5 is added dropwise in the solution and drips, is dripped with standard
Determine solution to be titrated to solution to become red from yellow to be terminal；
4) 30% ammonium fluoride of mass fraction is added, shakes up, stands 5-10min, and be heated to 30 DEG C~40 DEG C,
The complexing of aluminium and EDTA is destroyed, the EDTA with aluminium complexing is precipitated；
5) EDTA being precipitated again with Zinc standard solution titration, to measure the content of zinc and aluminium.
Wherein, the preparation method of 0.1mg/mL Zinc standard solution are as follows: weigh the benchmark zinc oxide in 800 DEG C of calcinations to constant
0.1g, it is cooling with 25mL hydrochloric acid heating for dissolving, it is transferred in 1L volumetric flask, is diluted with water to graduation mark, shake up rear spare.
The preparation method of HAc-NaAc buffer are as follows: weigh anhydrous sodium acetate 180g and be dissolved in a small amount of water, glacial acetic acid is added
15mL is diluted with water to 1L, shakes up rear spare.
The preparation method of 0.015mol/L EDTA standard solution are as follows: weigh 5.7g disodium ethylene diamine tetraacetate and burnt in 250mL
It in cup, is dissolved in water, is settled to 1000mL after cooling.
The present invention weigh 1g containing Zn content be 21%, the zinc sulfate that aluminium content is 5%, sulphur is carried out using the method in the present invention
Zinc and aluminum content tests in sour zinc, measure three times respectively；
The present invention also uses traditional measuring method to be determined the zinc sulfate for being 5% for 21%, aluminium content containing Zn content,
The step of traditional measuring method are as follows:
Sample to be tested 1g is weighed, 30% concentrated hydrochloric acid 10ml, 60% concentrated nitric acid 15ml is added in the sample, heating is steamed to wet salt, taken
Lower cooled to room temperature, sample is added water and stirred and is diluted to 100ml, prepares sample solution；Mass fraction 30% is added to be fluorinated
Ammonium shakes up, and stands 5-10min, and be heated to 30 DEG C~40 DEG C；It is that 30%HAc-NaAc buffer adjusts pH that mass fraction, which is added,
It is 5, then is titrated with 0.015mol/L EDTA standard solution, using xylenol orange as indicator, xylenol orange is added dropwise in the solution and refers to
Show that agent 3~5 is dripped, being titrated to solution to become red from yellow with standard titration solution is terminal.It measures respectively three times；It measures
Zn content and aluminium content see the table below:
1 aluminum and zinc assay result of table
In table: "/" expression cannot be detected.
As seen from the above table, the content of zinc and aluminium is respectively tested close to actual value, same sample in the sample through this method test
The standard deviation of aluminum and zinc between value is respectively 0.361%, 2%.Conventional method can not detect the content of aluminium, detect
The content of zinc is higher than actual value, illustrates that the content for the zinc that it is measured is the total content of aluminum and zinc.Shown by test result analysis
This method is used to measure the content of zinc and aluminium in zinc sulfate, sensitive, easy, stability is high, can satisfy production scene to sulphur
The test request of zinc and aluminium in sour zinc.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form,
Although the present invention has been disclosed as a preferred embodiment, however, it is not intended to limit the invention, any technology for being familiar with this profession
Personnel, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or repair
Decorations are the equivalent embodiment of equivalent variations, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments still fall within the range of technical solution of the present invention
It is interior.
Claims (6)
1. zinc, aluminum content tests method in a kind of industry ZnSO4, which comprises the following steps:
1) sample solution is prepared；
2) excessive EDTA standard solution is added into sample solution obtained by step 1), mixes, is cooled to room temperature after heating, carry out
Complex reaction obtains mixed solution；
3) the excessive ETDA titer of Zinc standard solution back titration is used, buffer is added and adjusts pH, is instruction with xylenol orange
Agent, with the ETDA of Zinc standard solution overtitration；
4) ammonium fluoride is added, destroys the complexing of aluminium and EDTA, the EDTA with aluminium complexing is precipitated；
5) EDTA being precipitated again with Zinc standard solution titration, to measure the content of zinc and aluminium.
2. zinc, aluminum content tests method in a kind of industry ZnSO4 as described in claim 1, which is characterized in that described to prepare sample
The step of product solution are as follows: weigh sample to be tested 1g, in the sample be added 30-35% concentrated hydrochloric acid 2~20ml, 60-70% concentrated nitric acid 2~
15ml, heating are steamed to wet salt, and cooled to room temperature is removed, and sample is added water and stirred and is diluted to 1000ml that sample is made is molten
Liquid.
3. zinc, aluminum content tests method in a kind of industry ZnSO4 as described in claim 1, which is characterized in that the step 2
Middle addition EDTA standard solution, after being boiled with soft fire 2min, is cooled to room temperature with flowing water immediately.
4. zinc, aluminum content tests method in a kind of industry ZnSO4 as claimed in claim 3, which is characterized in that the EDTA mark
The concentration of quasi- solution is 0.015mol/L.
5. zinc, aluminum content tests method in a kind of industry ZnSO4 as described in claim 1, which is characterized in that the buffer
For HAc-NaAc buffer, the volume of the buffer is 20-40mL, and the pH is 5-6, and the concentration of the Zinc standard solution is
0.1mg/mL。
6. zinc, aluminum content tests method in a kind of industry ZnSO4 as described in claim 1, which is characterized in that the step 4
In, mass fraction 30-40% ammonium fluoride is added, shakes up, stands 5-10min, and be heated to 30 DEG C~40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811345326.2A CN109187530A (en) | 2018-11-13 | 2018-11-13 | Zinc, aluminum content tests method in a kind of industry ZnSO4 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811345326.2A CN109187530A (en) | 2018-11-13 | 2018-11-13 | Zinc, aluminum content tests method in a kind of industry ZnSO4 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109187530A true CN109187530A (en) | 2019-01-11 |
Family
ID=64939419
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811345326.2A Pending CN109187530A (en) | 2018-11-13 | 2018-11-13 | Zinc, aluminum content tests method in a kind of industry ZnSO4 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109187530A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289507A (en) * | 2020-04-07 | 2020-06-16 | 晟通科技集团有限公司 | Method for detecting content of metal aluminum in aluminum slag |
| CN115060845A (en) * | 2022-05-20 | 2022-09-16 | 西部矿业股份有限公司 | Method for analyzing and detecting aluminum element in magnesium-aluminum hydrotalcite |
| CN115060845B (en) * | 2022-05-20 | 2024-05-03 | 西部矿业股份有限公司 | Analysis and detection method for aluminum element in magnesium aluminum hydrotalcite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
| CN105044275A (en) * | 2015-08-12 | 2015-11-11 | 成都光明光电股份有限公司 | Method for testing content of aluminum oxide in aluminum metaphosphate |
-
2018
- 2018-11-13 CN CN201811345326.2A patent/CN109187530A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
| CN105044275A (en) * | 2015-08-12 | 2015-11-11 | 成都光明光电股份有限公司 | Method for testing content of aluminum oxide in aluminum metaphosphate |
Non-Patent Citations (4)
| Title |
|---|
| 涂小红: "EDTA容量法测定锌合金中的铝量", 《福建分析测试》 * |
| 罗晓民等: "《皮革理化分析》", 30 September 2013, 中国轻工业出版社 * |
| 郭爽等: "硫酸锌中锌含量测定存在的问题及改进方法", 《中国饲料》 * |
| 钟国清等: "饲料级硫酸锌含量的测定方法研究", 《四川化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289507A (en) * | 2020-04-07 | 2020-06-16 | 晟通科技集团有限公司 | Method for detecting content of metal aluminum in aluminum slag |
| CN115060845A (en) * | 2022-05-20 | 2022-09-16 | 西部矿业股份有限公司 | Method for analyzing and detecting aluminum element in magnesium-aluminum hydrotalcite |
| CN115060845B (en) * | 2022-05-20 | 2024-05-03 | 西部矿业股份有限公司 | Analysis and detection method for aluminum element in magnesium aluminum hydrotalcite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dickman et al. | Colorimetric determination of phosphate | |
| CN102539511B (en) | Method for detecting content of bromine in fire retardant through automatic potentiometric titration | |
| CN102243177B (en) | Method for determining silicon dioxide in silicon carbide | |
| CN104458731A (en) | Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry | |
| WO2020233150A1 (en) | Method for calculating content of sodium chloride in edible salt | |
| CN108120797B (en) | Method for measuring SO in smoke gas by potentiometric titration2、SO3Method (2) | |
| CN104198484A (en) | Method for testing fluorine content in solution | |
| CN107132263A (en) | The method of testing of aluminium composition in aluminium etching solution | |
| CN104515826A (en) | Method for determination of tin content in tin-lead solder by complexometric titration method | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN109187530A (en) | Zinc, aluminum content tests method in a kind of industry ZnSO4 | |
| CN102735794A (en) | Method for determining nickel content in nickel-chromium-aluminum coated diatomite | |
| CN104914093B (en) | The method of testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal | |
| CN104655517A (en) | Measurement method of content of molybdenum in Mo-Al alloy | |
| CN104101576B (en) | A kind of method of nickel content in mensure steel | |
| CN105842388A (en) | Method for measuring sodium carbonate in sintering synergist through acid-base titration | |
| CN104062252A (en) | Method for measuring content of phosphorus pentoxide in glass | |
| CN109283287A (en) | The measuring method of antimony content in a kind of electrolytic antimony | |
| CN106645137A (en) | Testing method for metal-calcium-ion chelating capability of chelating acid | |
| CN106248667A (en) | A kind of Al-single crystal method in aluminium bronze | |
| CN102507568A (en) | Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt | |
| CN103940944A (en) | Method for detecting content of calcium oxide in limestone by using DBC (Dibromochloro)-arsenazo indicator | |
| CN108226375A (en) | Boric acid assay method in aqueous solution containing boric acid and zinc sulfate | |
| CN114280221A (en) | Method for detecting phosphorus content | |
| CN105067605A (en) | Method for continuously determining calcium content and iron content in limestone powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190111 |