CN108693170A - The analysis method of total chrome content in a kind of anodic oxidation solution - Google Patents
The analysis method of total chrome content in a kind of anodic oxidation solution Download PDFInfo
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- CN108693170A CN108693170A CN201810734020.XA CN201810734020A CN108693170A CN 108693170 A CN108693170 A CN 108693170A CN 201810734020 A CN201810734020 A CN 201810734020A CN 108693170 A CN108693170 A CN 108693170A
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- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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Abstract
The present invention relates to a kind of analysis methods of total chrome content in anodic oxidation solution, belong to basic scientific research technical field.The analysis method of total chrome content, includes the following steps in a kind of anodic oxidation solution:(1)Chromium standard solution is configured, chromium working curve is established;(2)Configuration oxidation solution determines oxidation solution used;(3)Inner mark solution is configured, and carries out internal standard detection and analysis;(4)With internal standard method, the standard solution different to 5 kinds of chromium contents carries out working curve measurement, and calculates its related coefficient.The invention has the advantages that:1, total chrome content in boric acid-sulphuric acid anodizing solution, easy to operate, saving reagent, raising high-volume anodic oxidation solution test solution analyze speed are detected using inductively coupled plasma emission spectrography, and has preferable precision and stability.2, with traditional analysis contrast test, for two groups of data without significant difference, this method systematic error is smaller.
Description
Technical field
The present invention relates to a kind of analysis methods of total chrome content in anodic oxidation solution, belong to basic scientific research technical field.
Background technology
The boric acid used in anode oxidation process-sulphuric acid anodizing solution total chrome content requirement is maintained in and is less than or equal to
Within the scope of 500ppm, for the detection of dynamic total chrome content, generally use is all potassium permanganate oxidation-hexichol phosphinylidyne at present
Two hydrazine spectrophotometry.The adjusting of pH is pretty troublesome in this method, but also can cause the loss of total chromium composition.
Invention content
The object of the present invention is to provide a kind of analysis methods of total chrome content in anodic oxidation solution, utilize inductive coupling etc.
Ion emission spectroscopy method obtains total chrome content in efficient, quick detection anodic oxidation solution.
To achieve the goals above, the present invention adopts the following technical scheme that:Total chrome content in a kind of anodic oxidation solution
Analysis method includes the following steps:
(1)Chromium standard solution is configured, chromium working curve is established:The standard solution of multiple elements such as aluminium, chromium, yttrium is prepared, light is carried out
Spectrum scanning, determines several glitch-free spectrum analysis line wavelength of chromium and Y element;
(2)Configuration oxidation solution determines oxidation solution used:Boric acid-sulphuric acid anodizing slot solution is configured, using pipette,
The analysis that 5 times, 10 times, 20 times extension rates are carried out to anodizing tank solution, determines appropriate dilutions multiple;
(3)Inner mark solution is configured, and carries out internal standard detection and analysis:Chromium concn is configured with Y element content difference and containing certain acid
5 kinds of standard solution of degree and each element investigate the sensitivity of chromium and Y element, determine analysis spectral line;In certain power, load
In range of flow and observed altitude, the I-c curves of 5 kinds of standard solution are measured, background equivalent concentration is calculated according to I-c curves
BEC and sensitivity K, obtains suitable load volume and observed altitude;
(4)With internal standard method, the standard solution different to 5 kinds of chromium contents carries out working curve measurement, and calculates its related coefficient;Profit
With above-mentioned working curve, blank solution is measured 10 times, preparation method detection limit;Chromium content detection is carried out to the tank liquor of preparation,
Each is measured 10 times, obtains relative standard deviation and the rate of recovery.
Preferably, in step(3)In, the power used is 600W-1300W.
Preferably, in step(3)In, current-carrying capacity ranging from 0.6-1.6mL/min.Preferably, the current-carrying capacity range
For 1.5mL/min.
Preferably, in step(3)In, observed altitude 11.0mm-15.0mm.
Preferably, in step(1)In, the chromium content of standard solution is 1mg/mL.
Compared with prior art, the present invention having the following advantages that:
1, total chrome content in boric acid-sulphuric acid anodizing solution, operation are detected using inductively coupled plasma emission spectrography
Easy, saving reagent, raising high-volume anodic oxidation solution test solution analyze speed, and have preferable precision and stability.
2, with traditional analysis contrast test, for two groups of data without significant difference, this method systematic error is smaller.
Description of the drawings
Fig. 1 is emission spectrometry flow chart compared with spectrophotometry in the embodiment of the present invention.
Specific implementation mode
1 couple of present invention is further described below in conjunction with the accompanying drawings:The analysis side of total chrome content in a kind of anodic oxidation solution
Method includes the following steps:
(1)Determine analysis spectral line range:1 workshop tank liquor concentration of solution and 2 workshop tank liquor concentration of solution and formula phase is respectively configured
Close substrate liquid prepares the standard solution of multiple elements such as aluminium, chromium, yttrium, carries out spectral scan, determines several of chromium and Y element
Glitch-free spectrum analysis line wavelength.
(2)The influence and selection of acidity:Using pipette, the analysis of 5 times, 10 times, 20 times extension rates is carried out to tank liquor, is determined
Appropriate dilutions multiple.
(3)The influence of matrix element:Using Matrix phase, the influence of matrix element is eliminated.It, can root due to being detection unit element
According to principle similar in ingredient, the chromium content of standard solution is set to 1mg/mL.
(4)Determine analysis spectral line:Configuration chromium concn is different with Y element content and contains certain acidity(According to content 1)
It determines)With 5 standard solution of each element, the sensitivity of chromium and Y element is investigated, determines analysis spectral line.
(5)Determine watt level:Under 600W-1300W power, measure(4)In 5 kinds of standard solution I-c curves, according to I-c
Curve calculates background equivalent concentration BEC and sensitivity K.
(6)The influence of atomized air flow rate:To 5 kinds of standard solution, within the scope of 0.6-1.6mL/min current-carrying capacities, it is bent to measure I-c
The sensitivity K and background equivalent concentration BEC of line, obtain suitable load volume.
(7)Observed altitude:Early period power and atomized air flow rate study on the basis of, research observed altitude in 11.0mm-
15.0mm is the I-c curves of 5 kinds of standard solution, measurement sensitivity K and background equivalent concentration BEC, obtains suitable observed altitude.
(8)Sample lifting capacity:Current-carrying capacity range is fixed on 1.5mL/min.
(9)The calculating of working curve and related coefficient:Based on previous work, fixed running parameter, using internal standard method,
The standard solution different to 5 kinds of chromium contents carries out working curve measurement, and calculates its related coefficient.
(10)Method detection limit:Using above-mentioned standard curve, blank solution is measured 10 times, preparation method detection limit.
(11)Accuracy and precision measure:Using internal standard method, chromium content detection is carried out to the tank liquor of preparation, each measures 10
It is secondary, obtain relative standard deviation and the rate of recovery.
Imitate the main ingredient 45g/l sulfuric acid of boric acid-sulphuric acid anodizing slot, 8 g/l boric acid prepare solution, time of repose
More than for 24 hours.The workshop tank liquor of solution 1 and solution 2 is detected, recovery of standard addition is full between 95.38%-102.88%
Sufficient measurement request.Concrete outcome is as follows:
1,1 tank liquor of solution
This experiment selection standard curve method, relative error is up to 5% or less.
2,2 tank liquor of solution
This experiment selection standard addition method, relative error is up to 5% or less.
3, tank liquor is prepared
For the preparation tank liquor of sulfuric acid 45g/l, 8 g/l of boric acid, the detection limit of measurement method.Tank liquor and reality are prepared by detection
Workshop tank liquor reaches bath maintenance needs, meets measurement request.
In conjunction with attached drawing 1 and the above, it can be seen that:Boric acid-is detected using inductively coupled plasma emission spectrography
Total chrome content in sulphuric acid anodizing solution, analysis that is easy to operate, saving reagent, raising high-volume anodic oxidation solution test solution
Speed, and have preferable precision and stability.With traditional analysis contrast test, two groups of data are without significant difference, we
Method systematic error is smaller.
Claims (6)
1. the analysis method of total chrome content in a kind of anodic oxidation solution, it is characterised in that:Include the following steps:
(1)Chromium standard solution is configured, chromium working curve is established:The standard solution of multiple elements such as aluminium, chromium, yttrium is prepared, light is carried out
Spectrum scanning, determines several glitch-free spectrum analysis line wavelength of chromium and Y element;
(2)Configuration oxidation solution determines oxidation solution used:Boric acid-sulphuric acid anodizing slot solution is configured, using pipette,
The analysis that 5 times, 10 times, 20 times extension rates are carried out to anodizing tank solution, determines appropriate dilutions multiple;
(3)Inner mark solution is configured, and carries out internal standard detection and analysis:Chromium concn is configured with Y element content difference and containing certain acid
5 kinds of standard solution of degree and each element investigate the sensitivity of chromium and Y element, determine analysis spectral line;In certain power, load
In range of flow and observed altitude, the I-c curves of 5 kinds of standard solution are measured, background equivalent concentration is calculated according to I-c curves
BEC and sensitivity K, obtains suitable load volume and observed altitude;
(4)With internal standard method, the standard solution different to 5 kinds of chromium contents carries out working curve measurement, and calculates its related coefficient;Profit
With above-mentioned working curve, blank solution is measured 10 times, preparation method detection limit;Chromium content detection is carried out to the tank liquor of preparation,
Each is measured 10 times, obtains relative standard deviation and the rate of recovery.
2. the analysis method of total chrome content in anodic oxidation solution according to claim 1, it is characterised in that:In step
(3)In, the power used is 600W-1300W.
3. the analysis method of total chrome content in anodic oxidation solution according to claim 1, it is characterised in that:In step
(3)In, current-carrying capacity ranging from 0.6-1.6mL/min.
4. the analysis method of total chrome content in anodic oxidation solution according to claim 3, it is characterised in that:The current-carrying
Measure ranging from 1.5mL/min.
5. the analysis method of total chrome content in anodic oxidation solution according to claim 1, it is characterised in that:In step
(3)In, observed altitude 11.0mm-15.0mm.
6. the analysis method of total chrome content in anodic oxidation solution according to claim 1, it is characterised in that:In step
(1)In, the chromium content of standard solution is 1mg/mL.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112629968A (en) * | 2020-12-09 | 2021-04-09 | 中国第一汽车股份有限公司 | Method for measuring cations in electrophoresis tank liquid |
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| US20070292991A1 (en) * | 2006-06-20 | 2007-12-20 | Lisa Edith Helberg | Method for quantification of analytes in a titanium, tin or silcon tetrachloride sample |
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| CN103257136A (en) * | 2013-04-12 | 2013-08-21 | 中国航空工业集团公司北京航空材料研究院 | Determination method for calcium, cobalt, chromium and iron in tungsten carbide |
| CN103995044A (en) * | 2014-05-26 | 2014-08-20 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette butt |
| CN107525799A (en) * | 2017-08-25 | 2017-12-29 | 广西德邦科技有限公司 | The method of chromium content in inductively coupled plasma mass spectrometry measure indium |
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2018
- 2018-07-06 CN CN201810734020.XA patent/CN108693170A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7273588B1 (en) * | 2003-07-17 | 2007-09-25 | Air Liquide America L.P. | Methods of sampling halosilanes for metal analytes |
| US20070292991A1 (en) * | 2006-06-20 | 2007-12-20 | Lisa Edith Helberg | Method for quantification of analytes in a titanium, tin or silcon tetrachloride sample |
| CN102759563A (en) * | 2012-06-26 | 2012-10-31 | 广东省潮州市质量计量监督检测所 | Method for determining chrominum content in edible gelatine |
| CN103257136A (en) * | 2013-04-12 | 2013-08-21 | 中国航空工业集团公司北京航空材料研究院 | Determination method for calcium, cobalt, chromium and iron in tungsten carbide |
| CN103995044A (en) * | 2014-05-26 | 2014-08-20 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette butt |
| CN107525799A (en) * | 2017-08-25 | 2017-12-29 | 广西德邦科技有限公司 | The method of chromium content in inductively coupled plasma mass spectrometry measure indium |
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| CN112629968A (en) * | 2020-12-09 | 2021-04-09 | 中国第一汽车股份有限公司 | Method for measuring cations in electrophoresis tank liquid |
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