CN1828268A - 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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- CN1828268A CN1828268A CN 200610043356 CN200610043356A CN1828268A CN 1828268 A CN1828268 A CN 1828268A CN 200610043356 CN200610043356 CN 200610043356 CN 200610043356 A CN200610043356 A CN 200610043356A CN 1828268 A CN1828268 A CN 1828268A
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- manganese
- standard solution
- atomic absorption
- manganese content
- cyclopentadiene
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- 239000011572 manganese Substances 0.000 title claims abstract description 69
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000012086 standard solution Substances 0.000 title claims description 67
- 238000010521 absorption reaction Methods 0.000 title claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 150000002576 ketones Chemical class 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 33
- CLLSOFHOYCGNJP-UHFFFAOYSA-N carbon monoxide cyclopenta-1,3-diene manganese Chemical compound [Mn].[C]=O.[C]=O.[C]=O.C1C=CC=C1 CLLSOFHOYCGNJP-UHFFFAOYSA-N 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 17
- 238000001953 recrystallisation Methods 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- IGMWKVKUUFVVJP-UHFFFAOYSA-N cyclopenta-1,3-diene;manganese Chemical compound [Mn].C1C=CC=C1 IGMWKVKUUFVVJP-UHFFFAOYSA-N 0.000 claims description 10
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 150000002170 ethers Chemical class 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 20
- 239000000523 sample Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 11
- 238000010790 dilution Methods 0.000 description 8
- 239000012895 dilution Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- DEIHRWXJCZMTHF-UHFFFAOYSA-N [Mn].[CH]1C=CC=C1 Chemical compound [Mn].[CH]1C=CC=C1 DEIHRWXJCZMTHF-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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), tool 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 outstanding look 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
| The consumption of 200mg/L manganese standard solution, ml | The content of manganese in the corresponding series standard solution, mg/L |
| 6.25 | 25 |
| 12.5 | 50 |
| 18.75 | 75 |
| 25 | 100 |
| Annotate: volatile because of ethanol, operation wants fast during the preparation ethanolic solution, and in time the stopper of volumetric flask is covered. | |
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 (8)
1, the method for preparing standard solution in a kind of determining manganese content using atomic absorption method is characterized in that: with cyclopentadiene tricarbonyl manganese as standard substance.
2,, it is characterized in that the preparation of standard solution comprises the following steps: to select for use the high-purity cyclopentadiene manganese tricarbonyl according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 1; The high-purity cyclopentadiene manganese tricarbonyl is dissolved in alcohols, ethers or the organic solvent of ketone obtains standard solution.
3, according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 2, it is characterized in that: the purity of cyclopentadiene tricarbonyl manganese is greater than 99.9%.
4, method according to preparing standard solution in the described determining manganese content using atomic absorption method of claim 3, it is characterized in that: 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, after filtration, the filtrate cooling, crystallization, filtration obtains 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%.
5, according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 2, it is characterized in that described organic solvent comprises: a kind of or several potpourris wherein in absolute ethyl alcohol, tetrahydrofuran, diethylene glycol dimethyl ether, the hexone.
6, according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 2, it is characterized in that: in standard solution, add hydrochloric acid.
7, according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 6, it is characterized in that: the mol ratio of hydrochloric acid addition HCl and Mn atom is 3～5: 1.
8, according to the method for preparing standard solution in the described determining manganese content using atomic absorption method of claim 6, 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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|---|---|---|---|
| CNB2006100433569A CN100458412C (en) | 2006-03-25 | 2006-03-25 | Method for preparing standard solution for determining manganese content using atomic absorption method |
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|---|---|---|---|
| CNB2006100433569A CN100458412C (en) | 2006-03-25 | 2006-03-25 | Method for preparing standard solution for determining manganese content using atomic absorption method |
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| Publication Number | Publication Date |
|---|---|
| CN1828268A true CN1828268A (en) | 2006-09-06 |
| CN100458412C CN100458412C (en) | 2009-02-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374540A (en) * | 2018-09-27 | 2019-02-22 | 阜阳师范学院 | A method for simultaneous determination of the content of chromium (VI) and manganese (VII) in a 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS63186131A (en) * | 1987-01-28 | 1988-08-01 | Nkk Corp | Device for direct analysis of manganese in molten metal using atomic absorption spectrometry |
| JP2000275172A (en) * | 1999-03-24 | 2000-10-06 | Nkk Corp | Atomic absorption spectrometry method and apparatus |
| CN1223600C (en) * | 2002-06-21 | 2005-10-19 | 山东东昌精细化工科技有限公司 | Process for refining cyclopentadiene manganese tricarbonylprocess |
| US20050009194A1 (en) * | 2003-07-08 | 2005-01-13 | Franklin Randall M. | Analytical method and device for determining metal concentration in liquid hydrocarbon matrices |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374540A (en) * | 2018-09-27 | 2019-02-22 | 阜阳师范学院 | A method for simultaneous determination of the content of chromium (VI) and manganese (VII) in a 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 |
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| CN100458412C (en) | 2009-02-04 |
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