CN109187847A - The measuring method of iron content in copper alloy - Google Patents
The measuring method of iron content in copper alloy Download PDFInfo
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- CN109187847A CN109187847A CN201811055934.XA CN201811055934A CN109187847A CN 109187847 A CN109187847 A CN 109187847A CN 201811055934 A CN201811055934 A CN 201811055934A CN 109187847 A CN109187847 A CN 109187847A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The present invention provides the measuring methods of iron content in an Albatra metal, comprising: a certain amount of sample is weighed in triangular flask, using HCl-H2O2Low-temperature heat dissolved samples, heat resolve residue H2O2；It is complete to copper ion reduction that metallic zinc is added by several times, eliminates interference；It boils and is filtered solution in triangular flask with absorbent cotton, add mixture of sulfuric phosphoric acid, indicator is added, stable purple is titrated to as terminal using potassium bichromate standard titration solution.According to the technical solution of the present invention, the interference of copper is eliminated as reducing agent by using metallic zinc, while iron is reduced to divalent, being formed by sediment can be easily separated and wash, can redox titration after separation interference.Operating process is shorter, easy to operate to be easily mastered, and quickly, detection efficiency is high for measurement.Reagent type is few, and dosage is small, energy saving.It is suitable in metallurgical industry the quick survey of iron in copper alloy.
Description
Technical field
The present invention relates to metallurgical analysis technical fields, in particular to the measuring method of iron content in an Albatra metal.
Background technique
The alloy that one or more of other elements are constituted is added using fine copper by matrix in copper alloy (copper alloy).Copper
Alloy is divided into many kinds, and the alloy as composed by copper and zinc is brass, and the alloy of copper and mickel is copper-nickel alloy, and bronze is copper and in addition to zinc
The alloy formed with the element other than nickel, mainly there is tin bronze, aluminium bronze etc., and red copper is the very high copper of copper content, other miscellaneous
Matter total content is below 1%.Iron has particularly important as one of copper alloy alloying element, the Accurate Determining of content
Effect.
In copper alloy the measurement of iron generally use sulfosalicylic acid method, Zeemen effect Electrothermo-atomic absorption spectrometry,
Na2EDTA titration, plasma emlssion spectrometry etc..Ammoniacal copper complex ion can be generated in copper, and the miscellaneous element such as zinc, aluminium is then formed
Precipitating, thus sulfosalicylic acid photometry is not suitable for the measurement of iron in such copper alloy；Zeemen effect Electrothermal atomic absorption spectrometry
Method is high for measurement trace iron accuracy, not applicable for the iron of high level；Na2EDTA titration needs to carry out extraction step
Suddenly, a large amount of organic reagents such as methylisobutylketone are used, toxicity is big.The large-scale instruments method such as plasma emission spectrum equipment cost is high,
Often the element of measurement high-content is unfavorable for the long-time service of instrument, needs by diluting step by step.
Summary of the invention
The present invention is directed to solve at least one of the technical problems existing in the prior art or related technologies.
For this purpose, the object of the present invention is to provide the measuring methods of iron content in an Albatra metal.
In view of this, technical solution of the present invention provides the measuring method of iron content in an Albatra metal, comprising: weigh
A certain amount of sample is in triangular flask, using HCl-H2O2Low-temperature heat dissolved samples, heat resolve residue H2O2；Gold is added by several times
It is complete to copper ion reduction to belong to zinc, eliminates interference；It boils and is filtered solution in triangular flask with absorbent cotton, add mixture of sulfuric phosphoric acid,
Indicator is added, stable purple is titrated to as terminal using potassium bichromate standard titration solution.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
1) simple, quick: this method is rapid assay methods, forms precipitating by using metallic zinc also native copper, was easy
Filter, while iron being restored, it is i.e. titratable after filtering.Determination step is few, and time-consuming short, determination efficiency is high.
2) accurately, stablize: this method use sampler-dissolving method can fast decoupled copper alloy sample, interference separation completely,
Redox reaction fast and stable, titration end-point discoloration is obvious to be easy observation, and measurement result is accurate.
3) energy conservation and environmental protection: method is quick, and only molten sample step uses electric hot plate heating, and energy consumption is few；Metallic zinc is added to restore
While separation interference, iron is restored, the type and dosage that reduce drug using other reducing agents, energy conservation and environmental protection are no longer needed to.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Specific embodiment
In order to be more clearly understood that aforementioned aspect of the present invention, feature and advantage, With reference to embodiment
The present invention is further described in detail.It should be noted that in the absence of conflict, embodiments herein and reality
The feature applied in example can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other than the one described here other modes, therefore, protection scope of the present invention is not by described below
Specific embodiment limitation.
The measuring method of iron content in the copper alloy of embodiment according to the present invention, comprising: weigh a certain amount of sample in three
In the bottle of angle, using HCl-H2O2Low-temperature heat dissolved samples, heat resolve residue H2O2；By several times be added metallic zinc to copper ion also
It is former complete, eliminate interference；It boils and is filtered solution in triangular flask with absorbent cotton, add mixture of sulfuric phosphoric acid, indicator is added, with weight
It is terminal that potassium chromate standard titration solution, which is titrated to stable purple,.
By the above method, the measuring method of iron content is had the following technical effect that in copper alloy
1) simple, quick: this method is rapid assay methods, forms precipitating by using metallic zinc also native copper, was easy
Filter, while iron being restored, it is i.e. titratable after filtering.Determination step is few, and time-consuming short, determination efficiency is high.
2) accurately, stablize: this method use sampler-dissolving method can fast decoupled copper alloy sample, interference separation completely,
Redox reaction fast and stable, titration end-point discoloration is obvious to be easy observation, and measurement result is accurate.
3) energy conservation and environmental protection: method is quick, and only molten sample step uses electric hot plate heating, and energy consumption is few；Metallic zinc is added to restore
While separation interference, iron is restored, the type and dosage that reduce drug using other reducing agents, energy conservation and environmental protection are no longer needed to.
Specific embodiment:
1 reagent and material
Dense HCl (density 1.19g/mL)
H2O2(mass fraction 30%)
Metallic zinc (solid)
Mixture of sulfuric phosphoric acid (the concentrated phosphoric acid volume ratio that the concentrated sulfuric acid and density that density is 1.84g/mL are 1.69g/mL is 2:3)
Diphenylamine sulfonic acid sodium salt indicator (concentration of aqueous solution of diphenylamine sulfonic acid sodium salt is 0.4%)
With potassium bichromate standard titration solution (C (1/6K2Cr2O7)=0.03000mol/L)
2 analytical procedures
2.1 sample size
Weigh sample 0.4000g
2.2 measurement
0.4000g sample is weighed in 300mL triangular flask, adds the dense HCl (density 1.19g/mL) of 15mL, is added dropwise by several times
H2O2(mass fraction 30%), in low-temperature heat dissolved samples on electric hot plate, after sample is completely dissolved, continues in triangular flask
Heating, which is boiled 3-4 minutes, makes H2O2It decomposes complete.It removes slightly cold, adds 40mL water, be heated to boiling.By several times be added metallic zinc to copper from
The color of son, which disappears and crosses, adds 0.5-1g, boils 3 minutes, is immediately filtered solution in another 300mL triangle with absorbent cotton
In bottle, former triangular flask and precipitating is eluted with water.Filtrate in triangular flask is diluted to 100mL, adding 8mL mixture of sulfuric phosphoric acid, (density is
The concentrated phosphoric acid volume ratio that the concentrated sulfuric acid and density of 1.84g/mL are 1.69g/mL is 2:3), 4 drop diphenylamine sulfonic acid sodium salt instructions are added
Agent (concentration of aqueous solution of diphenylamine sulfonic acid sodium salt is 0.4%), with potassium bichromate standard titration solution (C (1/6K2Cr2O7)=
0.03000mol/L) being titrated to stable purple is terminal.
The calculating of 3 analysis results
In formula:
C: potassium bichromate standard titration solution,
V: the volume of titration consumption potassium bichromate standard titration solution, mL
M: sample mass, g are weighed
M (Fe): the molal weight of Fe, 55.85g/mol
Sample analysis control
Table 1
The obtained rate of recovery of content it can be seen from upper table 1 using iron in this method measurement copper alloy is higher, measurement
Accurately.
This method, as reducing agent, eliminates the interference of copper by using metallic zinc, while iron is reduced to divalent, institute's shape
At sediment can be easily separated and wash, separation interference after can redox titration.Operating process is shorter, easy to operate to be easy
It grasps, quickly, detection efficiency is high for measurement.Reagent type is few, and dosage is small, energy saving.It is suitable in metallurgical industry in copper alloy
The quick measurement of iron.
Technical solution of the present invention is explained above, according to the technical solution of the present invention, by using metallic zinc as also
Former agent eliminates the interference of copper, while iron is reduced to divalent, and being formed by sediment can be easily separated and wash, separation interference
After can redox titration.Operating process is shorter, easy to operate to be easily mastered, and quickly, detection efficiency is high for measurement.Reagent type
Few, dosage is small, energy saving.It is suitable in metallurgical industry the quick survey of iron in copper alloy.
In the description of this specification, the description of term " one embodiment ", " some embodiments ", " specific embodiment " etc.
Mean that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one reality of the invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or reality
Example.Moreover, description particular features, structures, materials, or characteristics can in any one or more of the embodiments or examples with
Suitable mode combines.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (1)
1. the measuring method of iron content in an Albatra metal characterized by comprising
A certain amount of sample is weighed in triangular flask, using HCl-H2O2Low-temperature heat dissolved samples, heat resolve residue H2O2；By several times
It is complete to copper ion reduction that metallic zinc is added, eliminates interference；It boils and is filtered solution in triangular flask with absorbent cotton, add sulphur phosphorus
Nitration mixture is added indicator, is titrated to stable purple as terminal using potassium bichromate standard titration solution.
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| CN201811055934.XA CN109187847A (en) | 2018-09-11 | 2018-09-11 | The measuring method of iron content in copper alloy |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404991A (en) * | 2016-08-23 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Method for determination of iron in copper alloy |
| CN107462665A (en) * | 2017-07-07 | 2017-12-12 | 泉州众志金刚石工具有限公司 | The assay method of iron content in a kind of iron copper and tin ternary pre-alloyed powder |
-
2018
- 2018-09-11 CN CN201811055934.XA patent/CN109187847A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404991A (en) * | 2016-08-23 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Method for determination of iron in copper alloy |
| CN107462665A (en) * | 2017-07-07 | 2017-12-12 | 泉州众志金刚石工具有限公司 | The assay method of iron content in a kind of iron copper and tin ternary pre-alloyed powder |
Non-Patent Citations (3)
| Title |
|---|
| 中国人民共和国航空航天工业部: "《中国人民共和国航空航天工业部航空工业标准 HB5422.8》", 1 September 1989 * |
| 任乔森 等: "重铬酸钾滴定法测定自然铜中铁元素的含量", 《中国现代中药》 * |
| 林世光 主编: "《冶金化学分析》", 30 April 1981 * |
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Application publication date: 20190111 |