CN100458412C - Method for preparing standard solution for determining manganese content using atomic absorption method - Google Patents
Method for preparing standard solution for determining manganese content using atomic absorption method Download PDFInfo
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- CN100458412C CN100458412C CNB2006100433569A CN200610043356A CN100458412C CN 100458412 C CN100458412 C CN 100458412C CN B2006100433569 A CNB2006100433569 A CN B2006100433569A CN 200610043356 A CN200610043356 A CN 200610043356A CN 100458412 C CN100458412 C CN 100458412C
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Abstract
The method comprises: selecting high-pure clopentadiene manganese tricarbonyl to dissolve into the organic solvent with alcohol, ether or ketone. This invention can reduce testing cost.
Description
One, technical field
The field of the invention is the manganese element Determination on content in organism, organometallics and composition thereof.More particularly, manganese element in organism, organometallics and composition thereof (abbreviation Organic Manganese), its content can be measured with atomic absorption spectrography (AAS), needs preparing standard solution to compare in the mensuration process, the present invention relates to a kind of new standard solution compound method.
Two, background technology
Element manganese is widespread in nature, the method of manganese content has many kinds in the detection material, assay method (atomic absorption spectrophotometry) as potassium, sodium, iron, calcium, magnesium, manganese in the GB/T4634-1996 coal ash, GB/T 1506-2002 manganese ore manganese Determination on content (adopt potentiometric titration and ferrous ammonium sulfate titration), manganese content test method (atomic absorption spectrography (AAS)) etc. in manganese Determination on content method (atomic absorption spectrography (AAS)), the SH/T 0711-2002 gasoline in the ASTMD 3831-1994 gasoline.
Titrimetry is surveyed time-consuming, the effort of manganese content, and poor accuracy so employing now is few, is replaced by atomic absorption method gradually.The aas determination sample is easy, needn't ashing, and the sample pre-service is simple, becomes research and uses more analysis test method.
During aas determination element (metallic element) content, follow these steps to carry out:
(1) is equivalent to the standard solution or the standard solution series of 0.1～0.5 extinction reading according to the sensitivity of element to be measured preparation one.
(2) experiment condition of selection instrument is determined analytical approach.Calibration curve method, standard addition method, internal standard method, concentration readout method etc. are arranged usually.
(3) determine the preparation method of sample solution, and whether need to take to separate or the pre-treatment of enrichment; Determine whether to need to eliminate to disturb and the elimination way.The preparation sample solution, and be diluted to the concentration range that needs.
(4) absorbance of usefulness atomic absorption spectrometry standard solution, and the absorbance of sample solution.
(5) data processing calculates the content of element to be measured in the sample.
The preparation of standard solution is vital in The whole analytical process, and the accuracy of concentration of standard solution produces bigger influence with stability to test result.Want correct preparing standard solution, the at first standard substance that will choose (primary standard substance that is: contains element to be measured in this material, and can accurately learn the content of element to be measured in this material).For aas determination manganese element content, standard substance commonly used has high-purity manganese powder, high-purity manganese salt (as manganese sulfate) etc., will dissolve and preserve with nitric acid, hydrochloric acid during these standard substance preparing standard solutions, how the forms with aqueous solution exist, and be comparatively effective for the mensuration of inorganic manganese, and when being used to measure Organic Manganese, Organic Manganese to be decomposed, change into free manganese ion, measure with atomic absorption method again, complex operation, error are big, so be not suitable for the mensuration of Organic Manganese.Yao Cheng etc. have studied the method for manganese in the microemulsion sample introduction flame atomic absorption spectrometry mensuration cobalt iso-octoate, use lauryl sodium sulfate (SDS) as emulsifying agent, butanols is made assistant for emulsifying agent, solvent oil, water, SDS and butanols are mixed by a certain percentage, form stable microemulsion liquid, directly carry out flame atomic absorption spectrometry then and measure, thereby saved the processing of sample, method is easy, is used for the mensuration of cobalt iso-octoate manganese, has obtained satisfied result.But the method range of application is little, and different Organic Manganese will be screened different microemulsified prescriptions, has certain degree of difficulty.In order to measure Organic Manganese easily, there is the people to make the higher Organic Manganese standard solution of concentration (as being standard substance with sulfonic acid manganese among the ASTM D3831 abroad by specific process, the manganese standard solution of preparation 264.2mg/L), be diluted to standard solution or the standard solution series that is equivalent to 0.1～0.5 extinction reading with hexone (MIBK) during use, carry out sample manganese content analysis again.But this Organic Manganese standard solution costs an arm and a leg, and needs import, has increased analysis cost.
Three, summary of the invention
The invention provides the method for preparing standard solution in a kind of determining manganese content using atomic absorption method, its fundamental purpose is to be used for aas determination Organic Manganese content can measure Organic Manganese content more easily, reduces the analytical test expense.
Technical scheme of the present invention comprises:
With cyclopentadiene tricarbonyl manganese as standard substance.The preparation of standard solution comprises the following steps: to select for use the high-purity cyclopentadiene manganese tricarbonyl; The high-purity cyclopentadiene manganese tricarbonyl is dissolved in alcohols, ethers or the organic solvent of ketone obtains standard solution.
The purity of high-purity cyclopentadiene manganese tricarbonyl is more than 99.9%.Cyclopentadiene tricarbonyl manganese adopts repeatedly the mode of recrystallization to purify, promptly, the organic solvent that the cyclopentadiene tricarbonyl manganese crystal can be effectively dissolved in use dissolves cyclopentadiene tricarbonyl manganese, being heated to the cyclopentadiene tricarbonyl manganese crystal dissolves fully, filtrate cooling after filtration,, crystallization, filtration obtain the recrystallization material one time, through twice or twice above repeat above-mentioned recrystallization process, make purity and be the cyclopentadiene tricarbonyl manganese more than 99.9%.
The described organic solvent of preparing standard solution comprises: a kind of or several potpourris wherein in absolute ethyl alcohol, tetrahydrofuran, diethylene glycol dimethyl ether, the hexone.
Add hydrochloric acid in standard solution, the mol ratio of hydrochloric acid addition HCl and Mn atom is 3～5: 1.
The standard solution of preparation is diluted by different manganese content again, be made into series standard solution.
Method of the present invention is used for aas determination Organic Manganese content can measure Organic Manganese content more easily, reduces the analytical test expense.
Four, description of drawings
Do not have.
Five, embodiment
The invention will be further described below in conjunction with specific embodiment.
Cyclopentadiene tricarbonyl manganese (Cyclopentadienyl manganese tricarbonyl) is a kind of metal organic compound, molecular formula: C
5H
5Mn (CO)
3, molecular weight: 204.07, manganese content in the molecule: 26.921%, about 77 ℃ of fusing point is soluble in the organic solvent, and is water insoluble, in the dark stable.
Cyclopentadiene tricarbonyl manganese will pass through purification processes as standard substance, can adopt repeatedly the method for recrystallization (twice or twice above recrystallization) to purify, the recrystallization solvent for use be for can effectively dissolving the organic solvent of cyclopentadiene tricarbonyl manganese, comprises and is not limited to absolute ethyl alcohol, dimethylbenzene, dimethyl carbonate, butyl acetate, tetrahydrofuran, diethylene glycol dimethyl ether etc.Can obtain highly purified cyclopentadiene tricarbonyl manganese through recrystallization repeatedly, promptly purity reaches more than 99.9%.
The method of preparing standard solution of the present invention comprises the following step: with the cyclopentadiene tricarbonyl manganese of technical grade (for example: the product that Dongchang Shandong Fine Chemical Technology Co., Ltd produces) carry out repeatedly recrystallization and purify, the high-purity cyclopentadiene manganese tricarbonyl; The high-purity cyclopentadiene manganese tricarbonyl is dissolved in alcohols, ethers or the organic solvent of ketone; In solution, add small amount of hydrochloric acid,, obtain standard solution to improve the stability of solution; The standard solution of preparation is diluted by different manganese content again, be made into series standard solution.
The solvent that the present invention is used for preparing standard solution includes but not limited to a kind of or its potpourri of absolute ethyl alcohol, tetrahydrofuran, diethylene glycol dimethyl ether, hexone.
In the preferred embodiment of the present invention, the preparing standard solution solvent for use is absolute ethyl alcohol (liquid water content is less than 0.5%).
In another preferred embodiment of the present invention, the preparing standard solution solvent for use is a tetrahydrofuran.
In another preferred embodiment of the present invention, the preparing standard solution solvent for use is a diethylene glycol dimethyl ether.
In another preferred embodiment of the present invention, the preparing standard solution solvent for use is a hexone.
In another preferred embodiment of the present invention, manganese concentration is 1000mg/L in the standard solution of preparation.
In another preferred embodiment of the present invention, manganese concentration is 200mg/L in the standard solution of preparation.
Adopt method preparing standard solution of the present invention, when being used for working sample Organic Manganese content, sample dissolution dilution solvent for use should be identical with the solvent that standard solution adopts.
Accepted standard material cyclopentadiene tricarbonyl manganese among the present invention, unstable in solution, by in solution, adding watery hydrochloric acid, make manganese atom form new complex compound, obtain stable standard solution.
In another preferred embodiment of the present invention, the concentration of the added hydrochloric acid of standard solution of preparation is 1mol/L.
In another preferred embodiment of the present invention, the concentration of the added hydrochloric acid of standard solution of preparation is 0.5mol/L.
In another preferred embodiment of the present invention, the mol ratio of HCl and Mn atom is 3～5: 1 in the added hydrochloric acid of the standard solution of preparation.
Embodiment 1
Measure the manganese content in the manganese base RONA (MMT solution).
Take by weighing 50 gram technical grade cyclopentadiene tricarbonyl manganese crystal, use anhydrous alcohol solution, heating is filtered until dissolving fully, the filtrate cooling, crystallization, filter, obtain the recrystallization material one time, repeat said process with anhydrous alcohol solution again, up to making the recrystallization material three times, be the high-purity cyclopentadiene manganese tricarbonyl.
Accurately take by weighing high-purity cyclopentadiene manganese tricarbonyl 0.1858 gram (being accurate to 0.0001 gram), fully dissolve with the 150ml absolute ethyl alcohol, adding concentration is the hydrochloric acid 5ml of 1mol/L, solution is become near colourless by light yellow, at last solution is transferred in the volumetric flask of 250ml, be diluted to scale with absolute ethyl alcohol, fully shake up.Then join to such an extent that concentration is the standard solution of 200mg/L.
Get the volumetric flask of 4 50ml, press the manganese standard solution that the consumption shown in the table 1 adds 200mg/L, be diluted to scale, fully shake up with absolute ethyl alcohol.Then make series standard solution.
The serial manganese standard solution of table 1 preparation
Start atomic absorption spectrophotometer (AAS), select best condition of work,, select for use 279.5nm, spray into blank solution and series standard solution successively, obtain typical curve as analytical line with acetylene-air flame.
With the manganese content in this standard curve determination manganese base RONA (MMT solution).If prediction octane promoter manganese concentration is higher, 3～5 times of octane promoter (by quality) dilutions can be obtained dilute solution one time.Take by weighing dilute solution 0.125 gram one time, place the 100ml volumetric flask, add the 50ml absolute ethyl alcohol and fully shake up, adding concentration again is the hydrochloric acid 0.8ml of 1ml/L, solution will be faded near colourless by pale yellow, at last solution will be diluted to scale with absolute ethyl alcohol, get secondary dilution solution.Secondary dilution solution is fed the atomic absorption injector, from typical curve read the manganese concentration of this moment.Be calculated as follows the manganese content of RONA:
In the formula:
N---manganese concentration in the RONA, %;
V---secondary dilution liquor capacity, L;
A---extension rate;
C---manganese concentration from the secondary dilution solution that typical curve obtains, mg/L;
M---a dilute solution sample quality that takes by weighing, mg.
The arithmetic mean of getting twice replicate determination result is final measurement result.The result that result that the method records and stratographic analysis are measured matches.
The absolute ethyl alcohol of using in the example allows to contain a spot of water.
Embodiment 2
Measure manganese content (the manganese content 10～40mg/L) in the gasoline.
With a certain amount of high-purity cyclopentadiene manganese tricarbonyl of anhydrous alcohol solution, and adding hydrochloric acid is stablized, be made into the standard solution of manganese content 200mg/L, be diluted to the series standard solution that manganese content is respectively 10mg/L, 20mg/L, 30mg/L, 40mg/L with absolute ethyl alcohol again, absolute ethyl alcohol and series standard solution are sprayed into atomic absorption instrument successively, obtain linear typical curve.
With the not treated direct test of gasoline sample, the data that then record are more much lower than actual value.
Embodiment 3
Under the identical situation of other condition and embodiment 2, series standard solution is all diluted 5 times, and it is gasoline sample is first with 5 times of absolute ethyl alcohol dilutions, with appropriate hydrochloric acid stable after, use atomic absorption measuring manganese content again, its result is better than embodiment 2, but still has than large deviation, than actual value low 20%.
Embodiment 4
Under the identical situation of other condition and embodiment 2, series standard solution is all diluted 10 times, and with gasoline sample earlier with 10 times of absolute ethyl alcohol dilutions, with appropriate hydrochloric acid stable after, use manganese content in the atomic absorption measuring gasoline again, obtain satisfactory result.Manganese content actual value is 18mg/L in the gasoline, and measured value is in 18 ± 0.4mg/L, and deviation is less than 2.3%.
Embodiment 5
Under the identical situation of other condition and embodiment 4, change the solvent of standard solution into hexone (MIBK), with manganese content in the atomic absorption measuring gasoline, obtain satisfactory result.
Embodiment 6
Under the identical situation of other condition and embodiment 4, change the solvent of standard solution into diethylene glycol dimethyl ether, with manganese content in the atomic absorption measuring gasoline, obtain satisfactory result.
Claims (4)
1, the method for preparing standard solution in the manganese content process in a kind of aas determination organism, it is characterized in that comprising the following steps: selecting for use purity greater than 99.9% cyclopentadiene tricarbonyl manganese as standard substance, standard substance is dissolved in obtains standard solution in the organic solvent, and in standard solution, adding hydrochloric acid, described organic solvent is a kind of or several potpourris wherein in absolute ethyl alcohol, tetrahydrofuran, diethylene glycol dimethyl ether, the hexone.
2, method according to preparing standard solution in the manganese content process in the described aas determination organism of claim 1, it is characterized in that: cyclopentadiene tricarbonyl manganese adopts repeatedly the mode of recrystallization to purify, promptly, using effectively, the organic solvent of dissolving cyclopentadiene tricarbonyl manganese crystal dissolves cyclopentadiene tricarbonyl manganese, being heated to the cyclopentadiene tricarbonyl manganese crystal dissolves fully, after filtration, the filtrate cooling, crystallization, filtration obtains the recrystallization material one time, above repeat above-mentioned recrystallization process through twice, make purity for greater than 99.9% cyclopentadiene tricarbonyl manganese.
3, according to the method for preparing standard solution in the manganese content process in the described aas determination organism of claim 1, it is characterized in that: the mol ratio of hydrochloric acid addition HCl and Mn atom is 3～5: 1.
4, according to the method for preparing standard solution in the manganese content process in the described aas determination organism of claim 1, it is characterized in that: the standard solution of preparation is diluted by different manganese content again, be made into series standard solution.
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| CN100458412C true CN100458412C (en) | 2009-02-04 |
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| CN109374540B (en) * | 2018-09-27 | 2021-11-23 | 阜阳师范学院 | Method for determining specific determination conditions of chromium and manganese contents in solution |
| CN110895218A (en) * | 2019-12-24 | 2020-03-20 | 青岛海关技术中心 | Standard substance for detecting lead, manganese and iron contents in gasoline |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63186131A (en) * | 1987-01-28 | 1988-08-01 | Nkk Corp | Direct analysis instrument for manganese in molten metal by atomic absorption photometry |
| JP2000275172A (en) * | 1999-03-24 | 2000-10-06 | Nkk Corp | Atomic absorption analysis method and apparatus |
| CN1463976A (en) * | 2002-06-21 | 2003-12-31 | 东营南开精细化工科技有限公司 | Process for refining cyclopentadiene manganese tricarbonylprocess |
| CN1576826A (en) * | 2003-07-08 | 2005-02-09 | 乙基公司 | Analytical method and device for determining metal concentration in liquid hydrocarbon matrices |
-
2006
- 2006-03-25 CN CNB2006100433569A patent/CN100458412C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63186131A (en) * | 1987-01-28 | 1988-08-01 | Nkk Corp | Direct analysis instrument for manganese in molten metal by atomic absorption photometry |
| JP2000275172A (en) * | 1999-03-24 | 2000-10-06 | Nkk Corp | Atomic absorption analysis method and apparatus |
| CN1463976A (en) * | 2002-06-21 | 2003-12-31 | 东营南开精细化工科技有限公司 | Process for refining cyclopentadiene manganese tricarbonylprocess |
| CN1576826A (en) * | 2003-07-08 | 2005-02-09 | 乙基公司 | Analytical method and device for determining metal concentration in liquid hydrocarbon matrices |
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