CN103226073B - Microemulsion technology-based oil base mixing metal element standard solution preparation method - Google Patents
Microemulsion technology-based oil base mixing metal element standard solution preparation method Download PDFInfo
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- 239000012086 standard solution Substances 0.000 title claims abstract description 225
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 43
- 239000002184 metal Substances 0.000 title claims abstract description 39
- 238000002156 mixing Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 17
- 238000005516 engineering process Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000003921 oil Substances 0.000 claims abstract description 30
- 239000004094 surface-active agent Substances 0.000 claims abstract description 25
- 239000002480 mineral oil Substances 0.000 claims abstract description 22
- 235000010446 mineral oil Nutrition 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 26
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- 238000000034 method Methods 0.000 claims description 16
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- 229940113171 polysorbate 85 Drugs 0.000 claims description 13
- PRXRUNOAOLTIEF-WUOFIQDXSA-N sorbitan trioleate Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C\CCCCCCCC)C1OCC(O)C1OC(=O)CCCCCCC\C=C\CCCCCCCC PRXRUNOAOLTIEF-WUOFIQDXSA-N 0.000 claims description 13
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- 239000011701 zinc Substances 0.000 claims description 11
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
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- 239000011572 manganese Substances 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 9
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- 229910052748 manganese Inorganic materials 0.000 claims description 9
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- 229910052718 tin Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 8
- 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 claims description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 8
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052788 barium Inorganic materials 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
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- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 8
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 8
- 229910052793 cadmium Inorganic materials 0.000 claims description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
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- 238000004458 analytical method Methods 0.000 abstract description 6
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 26
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- 239000008236 heating water Substances 0.000 description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 11
- 229910017604 nitric acid Inorganic materials 0.000 description 11
- 239000011135 tin Substances 0.000 description 8
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
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- 239000003350 kerosene Substances 0.000 description 4
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- 239000010687 lubricating oil Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
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- 241001411320 Eriogonum inflatum Species 0.000 description 1
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- 238000002679 ablation Methods 0.000 description 1
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- 159000000021 acetate salts Chemical class 0.000 description 1
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- 239000011609 ammonium molybdate Substances 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a microemulsion technology-based oil base mixing metal element standard solution preparation method, which comprises the following steps: 1) respectively preparing single water base standard solutions, wherein concentrations of the single water base standard solution are 5000 mg/L; 2) mixing the taken standard solutions, and diluting to achieve a concentration of every element of 200 mg/L to obtain a mixed water base standard solution; and 3) uniformly mixing a mixed surfactant, an auxiliary surfactant, the mixed water base standard solution and white mineral oil, and carrying out ultrasound to carry out complete microemulsion to prepare the 10 mg/kg oil base mixing metal element standard solution. The mineral oil base metal multi-element mixing standard solution can be used for sample analysis according to standard methods ASTMD5189-09, ASTMD5708-11 and SN/T3189-2010. In addition, the microemulsion technology is adopted, and the inorganic salt with advantages of low price, high purity, more available selection types and the like is adopted to replace the oil-soluble metal salt so as to significantly reduce the oil base standard solution cost, preparing difficulty and types of the maximum mixing metal salts, and improve test accuracy.
Description
Technical field
The present invention relates to a kind of preparation method of the oil base hybrid metal elemental standards solution based on micro-emulsion technology.
Background technology
Generally all Determination of multiple metal elements is contained in crude oil, fuel oil and various product oil.These constituent contents are very low, general in mg/kg level, but it is very large on the impact of petroleum refining process and petroleum products matter, as nickel, vanadium etc. can destroy catalyst base skeleton structure, vanadium also can produce serious ablation to the blade of combustion gas turbine, sodium can make acidity of catalyst center poisoning, and the sediment blocking catalytic center of calcium, the existence of iron, copper also can have a negative impact to catalyst activity.Machine-building, communications and transportation, lubricating oil is applied widely in the numerous areas such as petroleum industry, its additive element (Mg, Mo, Ca, Zn, Ba, P etc.) the important indicator of content normally oil quality and usability, and wear and tear and pollution element (Ni in lubricating oil, Ti, Cr, Fe, Sn, A1, Mn, Si, Ph, Cu, Ag etc.) content be the important parameter of monitoring lubricating oil usability and the various lubricating machinery fault of prediction, particularly, in aerooil, the content of impurity element is directly connected to life-span and the aviation safety of engine, GJB135, GJB1263, GJB561, MIL-L-7808, the content of the standards such as MIL-L-23699 to these elements has considered critical.
Therefore, the quality evaluation of mensuration to Related product of these metal element contents is significant.Mensuration method for measuring conventional is at present based on inorganic method, by sample by high temperature ashing or clear up, be processed into inorganic aqueous solution, then import the spectrum Instrument measuring such as Atomic Absorption Spectrometer (AAS), inductive coupling plasma emission spectroscopy (ICP-AES).These class methods length consuming time and big for environment pollution, and directly organic solvent sampling method is by with organic solvent diluting sample dissolution, by special organic solvent sampling system introducing analytical instrument, can the content of the multiple oil soluble metal salt of Fast Measurement.The method is by many standards, and direct injected as organic in ASTM D5185-09 and GB/T17476-1998 measures A method in 22 elements such as aluminium, barium, ASTMD5708-11 and measures the employings such as iron, nickel, vanadium 3 kinds of elements.But above analysis all needs to use the higher organic metal standard items of price, to make Matrix Match, ensure the precision of analysis result.
The preparation of existing mineral oil based metal mixed standard solution, generally need to find suitable oil-soluble organic metal salt, as metal acetate salt or carboxylate etc., the mineral oil (or aviation kerosene) of certain specification is then used to dissolve and constant volume, for test after appropriate method is demarcated.The price of these organic salts is high, and purity has a definite limitation, and selectable leeway is few.Therefore, user often can only purchase the product of indivedual external specialized company at high price, as the Conostan that Canadian SCP SCIENCE company provides
tMseries organic metal oil ga(u)ge sample.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the oil base hybrid metal elemental standards solution based on micro-emulsion technology.
The technical solution used in the present invention is: a kind of preparation method of the oil base hybrid metal elemental standards solution based on micro-emulsion technology, comprise the following steps: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 2ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 200mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil are mixed, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 10mg/kg by ultrasonic for the potpourri of four.
A kind of preparation method of the oil base hybrid metal elemental standards solution based on micro-emulsion technology, comprise the following steps: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 5-10ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 500-1000mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil are mixed, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 25-50mg/kg by ultrasonic for the potpourri of four.
In step 3), described mixed surfactant is the potpourri of sorbester p37 and polysorbate85, and the mass ratio of sorbester p37 and polysorbate85 is 0.5-0.7, and the quality of mixed surfactant is the 25-40%wt of four potpourris.
In step 3), described cosurfactant is normal butyl alcohol, and the consumption of cosurfactant is the 1/8-1/12 of mixed surfactant.
In step 3), the method mixed four is: four potpourris are placed in turbine mixer mesoscale eddies mixing 15-30min.
In step 3), ultrasonic 30-60min.
The invention has the beneficial effects as follows: the mineral oil based metal mixture of multi-elements standard solution obtained by the present invention, can for the sample analysis by standard method ASTM D5189-09, ASTM D5708-11 and SN/T3189-2010, without the need to clearing up testing sample, the pre-treatment step such as constant volume, direct organic solvent sampling detects the content of Determination of multiple metal elements in crude oil, fuel oil, lubrication wet goods petrochemical industry sample.By contrast, because this patent have employed micro-emulsion technology, utilization has that price is low, purity is high and available kind is many etc. that advantage inorganic salts replace oil soluble metal salt, obviously can reduce the kind of the cost of oil base standard solution, configuration difficulty and maximum mixed metal salt, improve the precision of test.
Embodiment
A kind of preparation method of the oil base hybrid metal elemental standards solution based on micro-emulsion technology, comprise the following steps: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 2ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 200mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil vortex mixed is even, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 10mg/kg by ultrasonic for the potpourri of four.
In step 3), described mixed surfactant is the potpourri of sorbester p37 and polysorbate85, and the mass ratio of sorbester p37 and polysorbate85 is 0.5-0.7, and the consumption of mixed surfactant is the 25-40wt% of four potpourris; Described cosurfactant is normal butyl alcohol, and the quality of cosurfactant is the 1/8-1/12 of mixed surfactant.
If the element kind of testing less (less than 5 kinds and 5 kinds), then take following steps preparation standard solution: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 5-10ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 500-1000mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil vortex mixed is even, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 25-50mg/kg by ultrasonic for the potpourri of four.
In step 3), described mixed surfactant is the potpourri of sorbester p37 and polysorbate85, and the mass ratio of sorbester p37 and polysorbate85 is 0.5-0.7, and the consumption of mixed surfactant is the 25-40%wt of four potpourris; Described cosurfactant is normal butyl alcohol, and the quality of cosurfactant is the 1/8-1/12 of mixed surfactant.
The present invention utilizes microemulsion to have isotropic thermodynamic stability feature, with sorbester p37 and the composite mixed surfactant of polysorbate85, normal butyl alcohol is assistant for emulsifying agent, and make water-base metal mixed solution and mineral oil form microemulsion with vortex oscillation and ultrasonic means, with mineral oil based metal mixture of multi-elements standard solution obtained after the mixing of mineral oil constant volume, for the direct organic solvent sampling multiple metallic element analysis of inductance Coupled Plasma Spectroscopy instrument.Owing to adopting micro-emulsion technology, mineral oil based standard solution can be obtained with water-base metal salt, obviously can reduce the cost of test Plays reagent.
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1: the configuration of single-element standard solution
Aluminium (AL) standard solution: 5000.0mg/L, accurately take 5.0000g aluminium (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1, the i.e. hydrochloric acid of the 36.5wt% of 1 volume and the potpourri of 1 volume water, lower same), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Boron (B) standard solution: 5000.0mg/L, accurately takes 28.5968g boric acid, is placed in 1000mL beaker, covers table ware, add 500mL water, 30 DEG C are heated to dissolve, and dissolve completely and are cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Barium (Ba) standard solution: 5000.0mg/L, accurately takes 8.8931g barium chloride, adds the water-soluble solution of 500mL, dissolves completely and moves in 1000mL volumetric flask, be diluted with water to scale, mixing.
Beryllium (Be) standard solution: 5000.0mg/L, accurately take 5.0000g beryllium (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Bismuth (Bi) standard solution: 5000.0mg/L, accurately take 5.0000g bismuth (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL nitric acid (1+1, the nitric acid of the 65wt% of 1 volume and the potpourri of 1 volume water, lower same), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Cadmium (Cd) standard solution: 5000.0mg/L, accurately take 5.0000g cadmium (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 50mL water, 200mL nitric acid (1+1), 85 DEG C of heating water baths, dissolve completely and are cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Cobalt (Co) standard solution: 5000.0mg/L, accurately take 5.0000g cobalt (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL nitric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Chromium (Cr) standard solution: 5000.0mg/L, accurately take 5.0000g chromium (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Copper (Cu) standard solution: 5000.0mg/L, accurately take 5.0000g copper (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Iron (Fe) standard solution: 5000.0mg/L, accurately take 5.0000g iron (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Magnesium (Mg) standard solution: 5000.0mg/L, accurately take 5.0000g magnesium (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Manganese (Mn) standard solution: 5000.0mg/L, accurately take 5.0000g manganese (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL nitric acid (1+3, the i.e. 65wt% nitric acid of 1 volume and the potpourri of 3 volume water, lower same), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Nickel (Ni) standard solution: 5000.0mg/L, accurately take 5.0000g nickel (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL nitric acid (1+3), 85 DEG C of heating water baths, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Plumbous (Pb) standard solution: 5000.0mg/L, accurately take 5.0000g lead (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 50mL nitric acid (1+1), 85 DEG C of heating water baths, boil several minutes, drive away oxides of nitrogen, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Antimony (Sb) standard solution: 5000.0mg/L, accurately take 5.0000g metallic antimony (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 100mL hydrochloric acid (1+4, the i.e. hydrochloric acid of 1 volume 36.5wt% and the potpourri of 4 volume water), 85 DEG C of heating water baths, to dissolving completely, are cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Tin (Sn) standard solution: 5000.0mg/L, accurately take 5.0000g tin (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add the concentrated hydrochloric acid of the 36.5wt% of 100mL, 85 DEG C of heating water baths are to dissolving completely, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Titanium (Ti) standard solution: 5000.0mg/L, accurately take 5.0000g Titanium (massfraction is greater than 99.99%), be placed in 400mL polytetrafluoroethylene beaker, add 20mL hydrofluorite, drip 10mL nitric acid, 85 DEG C of heating water baths are to dissolving completely, cooling, add 20 mL sulfuric acid, be evaporated at 30-35 DEG C and emit sulfuric acid cigarette, then be cooled to room temperature, move in 1000mL volumetric flask, scale is diluted to, mixing with nitric acid (5+95, the i.e. potpourri of the nitric acid of the 65wt% of 5 volumes and the water of 95 volumes).
Vanadium (V) standard solution: 5000.0mg/L, accurately take 8.9258g vanadium pentoxide (massfraction is greater than 99.99%, is dried to constant weight in advance prior to 110 DEG C), be placed in 1000mL beaker, cover table ware, add the concentrated hydrochloric acid of the 36.5wt% of 100mL, drip 20wt% superoxol and be heated to dissolve completely, boil, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Zinc (Zn) standard solution: 5000.0mg/L, accurately take 5.0000g zinc (massfraction is greater than 99.99%), be placed in 1000mL beaker, cover table ware, add 200mL hydrochloric acid (1+1), 85 DEG C of heating water baths are to dissolving completely, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Potassium (K) standard solution: 5000.0mg/L, (massfraction is greater than 99.99% accurately to take 9.5334g potassium chloride, pre-prior to 500 DEG C of-600'C calcinations to constant weight), be placed in 1000mL beaker, add the water-soluble solution of 500mL, dissolve completely and move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Sodium (Na) standard solution: 5000.0mg/L, (massfraction is greater than 99.99% accurately to take 12.7105g sodium chloride, pre-prior to 500 DEG C of-600'C calcinations to constant weight), be placed in 1000mL beaker, add the water-soluble solution of 500mL, dissolve completely and move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Calcium (Ca) standard solution: 5000.0mg/L, (massfraction is greater than 99.99% accurately to take 12.4860g calcium carbonate, constant weight is dried in advance) at 110 DEG C, cover table ware, add 100mL hydrochloric acid (1+1), 85 DEG C of heating water baths are to dissolving, dissolve completely and be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Molybdenum (Mo) standard solution: 5000.0mg/L, (massfraction is greater than 99.99%, (NH accurately to take 9.2011g ammonium molybdate
4)
7mo
7o
244H
2o), add the water-soluble solution of 500mL, dissolve completely and move in 1000mL volumetric flask, be diluted with water to scale, mixing.
Embodiment 2: the preparation of complex element standard solution
According to the kind of required element, corresponding difference accurately draws list mark solution in 2mL embodiment 1 to the volumetric flask of 50mL, is diluted to scale mark, can obtains the mixed standard solution that concentration is 200mg/L with one-level water.
Embodiment 3: the preparation of oil base hybrid metal elemental standards solution
The concentration accurately measuring preparation in 2.5mL embodiment 2 is the water base standard solution of hybrid metal that 200mg/L contains Determination of multiple metal elements, (composite ratio is sorbester p37/polysorbate85=0.5 ~ 0.7 to 15.0g mixed surfactant sorbester p37+polysorbate85, mass ratio), 1.5g cosurfactant normal butyl alcohol in 50mL tool plug centrifuge tube (as precision be 0.001g electronic balance on, and deduct tare weight), finally add LUBKLEAR
tM90NF White Mineral Oil to gross mass is 50.00g.Build centrifugal bottle stopper, with in turbine mixer (as IKA MS3) potpourri vortex mixed 15 minutes, within ultrasonic 30 minutes, make the abundant microemulsified of mixing material, the transparent shape of potpourri, then obtain the mineral oil based metal mixed standard solution that concentration is 10mg/kg; The standard solution configured, is transferred to clean brown tool plug wide-mouth reagent bottle, keeps in Dark Place under room temperature, and for test, its term of validity is 6 ~ 9 months.
Checking example:
1 reagent and material
1.1 thinning agents: the alkane aromatic hydrocarbons mixed solvent (as aviation kerosene) not containing tested element.
1.2 mineral oil: the lube base oil not containing tested element or white oil (light-end products), as the LUBKLEAR that Lu Bo company of the U.S. produces
tMseries food level White Mineral Oil.
1.3 organic metal oil ga(u)ge samples: the organic metal oil standard specimen of mixing of chromium, copper, iron, magnesium, nickel, lead, vanadium, zinc multielement, concentration is 100mg/kg.The organic metal oil ga(u)ge sample S-21+K+Li+Sb that Conostan company of the U.S. provides.
1.4 Y Int Std: concentration is 1000mg/kg, Conostan company of the U.S. provides.
2 instruments
2.1 inductive coupling plasma emission spectrographs: the Thermo iCAP6500 of Thermo Fisher Scientific Inc. of the U.S., configures organic sampling system.
2.2 sample bottle 100 mL are with the PET bottle of screw top.
3. sampling and sample preparation
The mixed standard solution of the preparation flow configuration of mineral oil based metal mixture of multi-elements standard solution is prepared by micro-emulsion technology.
4 analytical procedures
The preparation of 4.1 inner mark solutions
Take a certain amount of Y Int Std (1.4) to be put in sample bottle (2.2), dilute 10 times in mass ratio with thinning agent, make this inner mark solution concentration be 100mg/kg.
The preparation of 4.2 standard solution
4.2.1 the preparation of blank solution: take mineral oil (1.2) as blank, add 1.0ml inner mark solution (4.1), with mineral oil: thinning agent=1:9(mass ratio) dilution ratio dilute, mix.
4.2.2 the preparation of standard working solution series: take serial organic metal oil ga(u)ge sample (1.3) in sample bottle, add 1.0ml inner mark solution (4.1), dilute with thinning agent again, with organic metal oil ga(u)ge sample: thinning agent=1:9(massfraction) dilution ratio dilute, obtain the standard working solution series of variable concentrations, various concentration of element in sample is dropped in the range of linearity of standard working curve, and fully shakes up rear sealing preservation.
4.2.3 the preparation of sample solution: take the sample after abundant homogenizing process in sample bottle, add 1.0ml inner mark solution (4.1) again with thinning agent dilution with sample: thinning agent=1:9(mass ratio) dilution ratio dilute, and fully shake up rear sealing preservation.
4.3 instruments prepare
4.3.1 instrument condition: with reference to the operating conditions with organic solvent sample introduction provided in instrument manual, set up the instrument optimum operation condition that its choice for use diluting solvent measures.
4.3.2 operating parameter is selected: set up suitable instrumentation condition of work, so that can measurement target element.These parameters comprise: element, wavelength, integral time and Internal standard correction methods.Recommend to measure wavelength see table 1, typical operating parameter is see table 2.
The mensuration wavelength of each element of table 1
| Element | Recommend wavelength, nm |
| Chromium | 267.7 283.5 |
| Copper | 324.7 327.3 |
| Iron | 238.2 259.9 |
| Magnesium | 279.0 279.5 |
| Nickel | 341.4 221.6 |
| Plumbous | 261.4 283.3 |
| Vanadium | 292.4 310.2 |
| Zinc | 213.8 |
| Yttrium | 371.0 |
The operating parameter of table 2 inductive coupling plasma emission spectrograph
| Project | Running parameter |
| Power (KW) | 1.35 |
| Cooling gas flow (L/min) | 18.0 |
| Assisted gas flow (L/min) | 1.0 |
| Atomization gas flow (L/min) | 0.50 |
| Oxygen flow (L/min) | 0.15 |
| Pump speed (rpm) | 30 |
| Long wave integral time (s) | 10 |
| Shortwave integral time (s) | 5 |
| Integral number of times | 2 |
Cr, Cu, Fe, Mg, Ni, Pb, V, Zn mixed standard solution of this patent method preparation pressed by table 3., the test result take aviation kerosene as solvent and yttrium (371.0nm) being internal standard element
Table 4. is pressed this patent method preparation GSB04-1767-2004ICP and is analyzed with (24 element) mixed standard solution, the test result take aviation kerosene as solvent and yttrium (371.0nm) being internal standard element
Significant difference inspection (the t method of inspection: check in corresponding t by table of table 5.3 kind of standard solution test value
a,fvalue, if t<t
a,f, between test value, there is no conspicuousness error)
Claims (2)
1. the preparation method based on the oil base hybrid metal elemental standards solution of micro-emulsion technology, it is characterized in that: comprise the following steps: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 2ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 200mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil are mixed, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 10mg/kg by ultrasonic for the potpourri of four,
Wherein, in step 3), described mixed surfactant is the potpourri of sorbester p37 and polysorbate85, and the mass ratio of sorbester p37 and polysorbate85 is 0.5-0.7, and the consumption of mixed surfactant is the 25-40% wt of four potpourris;
In step 3), described cosurfactant is normal butyl alcohol, and the quality of cosurfactant is the 1/8-1/12 of mixed surfactant;
In step 3), the method mixed four is: four potpourris are placed in turbine mixer mesoscale eddies mixing 15-30min;
In step 3), ultrasonic 30-60min.
2. the preparation method based on the oil base hybrid metal elemental standards solution of micro-emulsion technology, it is characterized in that: comprise the following steps: 1) configure single water base standard solution respectively for following often kind of element: aluminum standard solution, boron standard solution, barium standard solution, beryllium standard solution, bismuth standard solution, cadmium standard solution, cobalt standard solution, chromium standard solution, copper standard solution, iron standard solution, magnesium standard solution, manganese standard solution, nickel standard solution, plumbous standard solution, antimony standard solution, tin standard solution, titanium standard solution, vanadium standard solution, Zinc standard solution, potassium standard solution, sodium standard solution, calcium standard solution, molybdenum standard solution, the concentration of single water base standard solution is 5000mg/L, 2) for the element that will test, take the single water base standard solution 5-10ml of respective element respectively, being mixed and be diluted to often kind of concentration of element by the standard solution of taking is 500-1000mg/L, obtains mixed water base standard solution, 3) the mixed water base standard solution of mixed surfactant, cosurfactant, 2.5ml, White Mineral Oil are mixed, four gross masses are 50g, its abundant microemulsified is made again, i.e. the oil base hybrid metal elemental standards solution of obtained 25-50mg/kg by ultrasonic for the potpourri of four,
Wherein, in step 3), described mixed surfactant is the potpourri of sorbester p37 and polysorbate85, and the mass ratio of sorbester p37 and polysorbate85 is 0.5-0.7, and the consumption of mixed surfactant is the 25-40% wt of four potpourris;
In step 3), described cosurfactant is normal butyl alcohol, and the quality of cosurfactant is the 1/8-1/12 of mixed surfactant;
In step 3), the method mixed four is: four potpourris are placed in turbine mixer mesoscale eddies mixing 15-30min;
In step 3), ultrasonic 30-60min.
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