CN103424403A - Quick bath measuring method of Zn in aluminum alloy - Google Patents
Quick bath measuring method of Zn in aluminum alloy Download PDFInfo
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- CN103424403A CN103424403A CN2013102912873A CN201310291287A CN103424403A CN 103424403 A CN103424403 A CN 103424403A CN 2013102912873 A CN2013102912873 A CN 2013102912873A CN 201310291287 A CN201310291287 A CN 201310291287A CN 103424403 A CN103424403 A CN 103424403A
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- aluminium alloy
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 42
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004448 titration Methods 0.000 claims abstract description 21
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 20
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 11
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 11
- 238000005259 measurement Methods 0.000 claims abstract description 11
- 229960004011 methenamine Drugs 0.000 claims abstract description 11
- 239000012086 standard solution Substances 0.000 claims abstract description 11
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 6
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 6
- 208000030208 low-grade fever Diseases 0.000 claims description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 3
- 229940012189 methyl orange Drugs 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001431 copper ion Inorganic materials 0.000 abstract description 3
- 238000010668 complexation reaction Methods 0.000 abstract 1
- 230000000873 masking effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 10
- 230000000536 complexating effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 150000008040 ionic compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of chemical measuring methods of metallic elements, and provides a quick bath measuring method of Zn in aluminum alloy. The method comprises the following steps: dissolving a sample by mixed acid, and using sodium fluoride to realize complexation with Fe <3+>, Al <3+> and thiourea masking copper ions to reduce interference of impurity elements to determination; adding hexamethylene tetramine to buffer the acid-base property of solution; using xylenol orange as an indicator, using EDTA standard solution to perform titration, measuring percentage content of the Zn according to the titration size, performing measurement for 3 times and obtaining an average value. According to the method provided by the invention, the content of Zn in the aluminium alloy can be accurately measured; the detection time is 15 min, so that 1/2 time is saved compared with a national standard (GB/T20975.8-2008) method I taking 30 min for measuring; the method is further suitable for quick bath analysis, and required devices are simple, convenient and low in cost.
Description
Technical field
The invention belongs to the chemistry in detecting technical field of metallic element, be specifically related to the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold.
Background technology
It is high that aluminium alloy A420 material has tensile strength, and damping and amortization is good, and the advantages such as wear resistance is good, low cost of manufacture are used as a kind of high performance new engineering material and are widely used.Yet, due to raw-material difference, the difference of production technology causes in alumin(i)um zinc alloy impurity elements such as containing Si, Cu, Mg, Fe, Ca, Sn, and these impurity elements have very large interference to the Zn in the Accurate Determining alloy, if by colorimetric method for determining Zn ion, its poor reproducibility.And measure by GB (GB/T20975.8-2008) method one, need to process with strong-base anion-exchange resin, the loaded down with trivial details and length consuming time of testing procedure, be unfavorable for both analysis; GB (GB/T20975.8-2008) method two is measured, and need to measure with the inductively coupled plasma atomic emission spectrometry instrument, and the instrument and equipment expense that the method needs is high, the maintaining difficulty, and testing cost is higher.
Summary of the invention
The present invention, in order to measure effectively, accurately and cheaply fast the content of Zn in aluminium alloy, provides the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold.
The present invention is realized by following technical scheme: the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold, and it is characterized in that: concrete steps are as follows:
(1) take alloy sample in the 300ml conical flask, add the mixed-acid dissolution alloy sample, and then be evaporated to dry;
(2) add 50ml water, the 1.5g sodium fluoride, add the 10ml thiocarbamide after dissolving, drips 3-4 and drip methyl orange, and solution is aobvious red;
(3) with the titration of hexamethylene tetramine solution, solution is become colorless by redness, after minim, determine 10ml hexamethylene tetramine solution, making solution PH is 5-6, aobvious red;
(4) add 15 xylenol orange indicator, the solution pinkiness, with the titration of EDTA standard solution, when solution is become colorless as titration end-point by redness, record the volume of the EDTA standard solution that titration consumes, and calculates the percentage composition of Zn by following formula:
In formula: the standard EDTA that C is 0.01mol/L;
V
EDTAVolume for the quota of expenditure EDTA of titration institute solution;
M by the quality of survey aluminium alloy.
Acid mixture used is that the red fuming nitric acid (RFNA) by the HCl of 150ml 1:1 and 25ml 70% mixes, and consumption is 8-15ml; During dissolved samples, require low-grade fever to dissolve, solution temperature is 30-50 ℃.Thiourea solution concentration used is 10%, and methyl orange solution concentration is 0.1%, and the hexamethylene tetramine solution concentration is 30%, and the xylenol orange solution concentration is that 0.5%, EDTA concentration of standard solution is 0.01mol/L, and Specimen Determination is got its mean value 3 times.
Outstanding advantages of the present invention is: detection method of the present invention has short, testing result accurate and effective detection time, low cost and other advantages.
Adopting detection method of the present invention detection time is 15min, than the minute 30min of GB (GB/T20975.8-2008) method one, has saved half the time, is suitable for carrying out both analysis.In testing process, due to the HCl of the 1:1 that has adopted 150ml, the red fuming nitric acid (RFNA) acid mixture of 25ml 70%, after alloy sample is dissolved, evaporation is dry again, and metallic elements all in alloy is existed with the form of ionic compound crystal, play a part to transform sample, and do not affect measurement result.The dissolution time of metallic element in the alloy sample has been saved in the use of acid mixture, has also saved the naturally cooling time of solution, therefore, has greatly shortened the needed time of testing process.The Fe that adopted the sodium fluoride complexing
3+, Al
3+Copper ion has been sheltered in adding of thiocarbamide, has reduced the interference of these impurity elements to the Zn in the Accurate Determining alloy, therefore, adopt the method for the invention can not affect the testing result of sample, its testing result is consistent with GB (GB/T20975.8-2008) method two testing result.When being applicable to not possess the service condition of the equipment such as Atomic Emission Spectrometer AES, detection method of the present invention uses.
Embodiment
In the Fast Measurement aluminium alloy of a kind of stokehold of the present invention, the ultimate principle of the method for Zn is as follows: at first sample, through mixed-acid dissolution, makes metallic elements all in alloy exist with the form of ionic compound crystal; Then use sodium fluoride complexing Fe
3+, Al
3+, thiocarbamide shelters copper ion, thereby reduce the interference of these impurity elements to measuring; Add hexamethylene tetramine to be cushioned the Acidity of Aikalinity of solution, PH is controlled between 5-6; Make indicator with xylenol orange, with the titration of EDTA standard solution, according to the titration volume of EDTA standard solution, calculate the percentage composition of its Zn, measure 3 times and get its mean value.
Below by embodiment, the present invention is described in detail, concrete steps are as follows:
1. accurately take the 0.1g alloy sample in the 300ml conical flask, add 10ml acid mixture and carry out the low-grade fever dissolving, solution temperature is 30-50 ℃, and then be evaporated to dry, metallic elements all in alloy is existed with the form of ionic compound crystal, and the HCl that wherein acid mixture is 150ml 1:1 and the red fuming nitric acid (RFNA) of 25ml 70% mix;
2. add 50ml water, the 1.5g sodium fluoride, add the thiourea solution that 10ml concentration is 10% after dissolving, drips 3-4 and drip the methyl orange that concentration is 0.1%, and solution is aobvious red;
3. make with 30% hexamethylene tetramine solution titration that solution is red to disappear just, solution is colourless, excessive titration 10ml hexamethylene tetramine then, and solution is aobvious red, and now solution PH is 5-6;
4. the xylenol orange indicator that adds 15 0.5%, make the solution pinkiness, with the titration of EDTA standard solution, solution is stopped by the redness titration that becomes colorless, record the volume of the EDTA standard solution that titration consumes, calculate the percentage composition of Zn by following formula, measure 3 times and get its mean value:
In formula: the standard EDTA that C is 0.01mol/L;
V
EDTAVolume for the quota of expenditure EDTA of titration institute solution;
M by the quality of survey aluminium alloy.
In present embodiment, in order to improve the selectivity of EDTA, guarantee to measure precision, the inventive method is controlled following influence factor:
(1) control of complexing acidity: owing to selecting acid mixture to carry out dissolution sample, add hexamethylene tetramine solution, pH value is transferred to the best color change interval 5-6 of xylenol orange indicator, and makes solution there is certain surge capability (because can discharge H when EDTA and complexing of metal ion
+).
(2) during dissolution sample, use the low-grade fever of 30-50 ℃ to dissolve, be for sample is dissolved fully, and saved the naturally cooling time of solution.
(3) selecting of indicator and screening agent: because Zn element and EDTA complexing are under solutions of weak acidity, so select the xylenol orange indicator proper.Due to Fe
3+, Al
3+, Cu
2+Deng impurity element, mensuration is had to very large interference, therefore by the method for sheltering, reduce the concentration of interfering ion, improve the accuracy of titration.
Gather from the 1st stove and the 3rd stove sample produced, every stove sample is divided into two parts, and a the inventive method of using is measured, and another part adopts GB (GB/T20975.8-2008) method two to measure by Zhengzhou light metal inspection center of country.The testing result comparative analysis is in Table 1.
Table 1: Analysis of test results
| Sample number into spectrum | Test item | The inventive method measured result | Zhengzhou light metal inspection center of country is detected | Absolute error | Relative error |
| 1 | Zn | 4.49 | 4.54 | 0.05 | 1.10% |
| 3 | Zn | 4.30 | 4.27 | 0.03 | 0.70% |
By table 1, can find out, two kinds of method measured result absolute errors are less than 0.06, all meet the different experiments chamber and detect error criterion, illustrate the method for the invention can the Accurate Determining aluminium alloy in the content of Zn.Adopting detection method of the present invention detection time is 15min, minute 30min than GB (GB/T20975.8-2008) method one has saved half the time, therefore the method for the invention also is suitable for carrying out the express-analysis of stokehold, and device therefor is simple, convenient, and cost is lower.
Claims (4)
1. the method for Zn in a stokehold Fast Measurement aluminium alloy, it is characterized in that: concrete steps are as follows:
(1) take alloy sample in the 300ml conical flask, add the mixed-acid dissolution alloy sample, and then be evaporated to dry;
(2) add 50ml water, the 1.5g sodium fluoride, add the 10ml thiocarbamide after dissolving, drips 3-4 and drip methyl orange, and solution is aobvious red;
(3) with the titration of hexamethylene tetramine solution, solution is become colorless by redness, after minim, determine 10ml hexamethylene tetramine solution, making solution PH is 5-6, aobvious red;
(4) add 15 xylenol orange indicator, the solution pinkiness, with the titration of EDTA standard solution, when solution is become colorless as titration end-point by redness, record the volume of the EDTA standard solution that titration consumes, and calculates the percentage composition of Zn by following formula:
In formula: the standard EDTA that C is 0.01mol/L;
V
EDTAVolume for the quota of expenditure EDTA of titration institute solution;
M by the quality of survey alloy.
2. the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold according to claim 1 is characterized in that: acid mixture used is that the red fuming nitric acid (RFNA) by the HCl of 150ml 1:1 and 25ml 70% mixes, and consumption is 8-15ml.
3. the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold according to claim 1 is characterized in that: during dissolved samples, require low-grade fever to dissolve, solution temperature is 30-50 ℃.
4. the method for Zn in the Fast Measurement aluminium alloy of a kind of stokehold according to claim 1, it is characterized in that: thiourea solution concentration used is 10%, methyl orange solution concentration is 0.1%, the hexamethylene tetramine solution concentration is 30%, the xylenol orange solution concentration is that 0.5%, EDTA concentration of standard solution is 0.01mol/L.
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| CN201310291287.3A CN103424403B (en) | 2013-07-11 | 2013-07-11 | The method of Zn in the Fast Measurement aluminium alloy of a kind of stokehold |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792600A (en) * | 2015-04-22 | 2015-07-22 | 西安热工研究院有限公司 | Etchant for testing overtemperature phase change structure of 9-12% Cr martensite heat-resistant steel |
| CN105181691A (en) * | 2015-09-29 | 2015-12-23 | 聊城市鲁西化工工程设计有限责任公司 | Detection method for content of zinc in benzene hydrogenation catalyst |
| CN109358056A (en) * | 2018-12-26 | 2019-02-19 | 西南铝业（集团）有限责任公司 | A method of 7050 zinc in aluminium alloy contents of measurement |
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| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
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Non-Patent Citations (4)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792600A (en) * | 2015-04-22 | 2015-07-22 | 西安热工研究院有限公司 | Etchant for testing overtemperature phase change structure of 9-12% Cr martensite heat-resistant steel |
| CN105181691A (en) * | 2015-09-29 | 2015-12-23 | 聊城市鲁西化工工程设计有限责任公司 | Detection method for content of zinc in benzene hydrogenation catalyst |
| CN105181691B (en) * | 2015-09-29 | 2018-09-21 | 聊城市鲁西化工工程设计有限责任公司 | The detection method of Zn content in benzene hydrogenating catalyst |
| CN109358056A (en) * | 2018-12-26 | 2019-02-19 | 西南铝业（集团）有限责任公司 | A method of 7050 zinc in aluminium alloy contents of measurement |
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| CN103424403B (en) | 2015-11-18 |
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Effective date of registration: 20240319 Address after: 032300 South Cao village, Wutong Town, Xiaoyi, Lvliang, Shanxi Patentee after: XIAOYI DONGYI MAGNESIUM INDUSTRY Co.,Ltd. Country or region after: Zhong Guo Address before: 032308 South Cao village, Wutong Town, Xiaoyi, Lvliang, Shanxi Patentee before: SHANXI DONGYI COAL ALUMINUM GROUP Co.,Ltd. Country or region before: Zhong Guo |