CN105092570A - Method for continuously measuring contents of calcium and magnesium in silicon, calcium, barium and magnesium alloy - Google Patents
Method for continuously measuring contents of calcium and magnesium in silicon, calcium, barium and magnesium alloy Download PDFInfo
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- 239000011575 calcium Substances 0.000 title claims abstract description 45
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000011777 magnesium Substances 0.000 title claims abstract description 24
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 21
- 229910000600 Ba alloy Inorganic materials 0.000 title abstract description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 4
- 239000010703 silicon Substances 0.000 title abstract description 4
- 229910000882 Ca alloy Inorganic materials 0.000 title abstract 3
- 229910000861 Mg alloy Inorganic materials 0.000 title abstract 3
- 229910000676 Si alloy Inorganic materials 0.000 title abstract 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 31
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 10
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960002378 oftasceine Drugs 0.000 claims abstract description 8
- 239000012085 test solution Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 5
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 5
- 239000012086 standard solution Substances 0.000 claims description 29
- 239000000523 sample Substances 0.000 claims description 27
- 229910008045 Si-Si Inorganic materials 0.000 claims description 16
- 229910006411 Si—Si Inorganic materials 0.000 claims description 16
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 8
- 235000019504 cigarettes Nutrition 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000012490 blank solution Substances 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 244000061458 Solanum melongena Species 0.000 claims description 5
- 230000008034 disappearance Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 4
- 238000004448 titration Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 3
- SXYCCJAPZKHOLS-UHFFFAOYSA-N chembl2008674 Chemical compound [O-][N+](=O)C1=CC=C2C(N=NC3=C4C=CC=CC4=CC=C3O)=C(O)C=C(S(O)(=O)=O)C2=C1 SXYCCJAPZKHOLS-UHFFFAOYSA-N 0.000 abstract description 2
- 235000009328 Amaranthus caudatus Nutrition 0.000 abstract 1
- 240000001592 Amaranthus caudatus Species 0.000 abstract 1
- XWROUVVQGRRRMF-UHFFFAOYSA-N F.O[N+]([O-])=O Chemical compound F.O[N+]([O-])=O XWROUVVQGRRRMF-UHFFFAOYSA-N 0.000 abstract 1
- 235000012735 amaranth Nutrition 0.000 abstract 1
- 239000004178 amaranth Substances 0.000 abstract 1
- 230000003139 buffering effect Effects 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000000391 smoking effect Effects 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 19
- 239000010959 steel Substances 0.000 description 19
- 229910052782 aluminium Inorganic materials 0.000 description 17
- 239000004411 aluminium Substances 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 16
- 238000009628 steelmaking Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910001021 Ferroalloy Inorganic materials 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229920001617 Vinyon Polymers 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 230000003412 degenerative effect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013215 result calculation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for continuously measuring contents of calcium and magnesium in silicon, calcium, barium and magnesium alloy. The method comprises the following steps: adding a silicon, calcium, barium and magnesium alloy test sample into one flask, taking the other flask as a blank contrast, respectively adding a nitric acid-hydrofluoric acid mixed solution to dissolve the test sample, adding perchloric acid for smoking, then adding hydrochloric acid to dissolve salts, transferring the test solution into a large-capacity bottle, diluting to the scale, respectively taking two groups of quantitative solutions from the volume-fixed solution into the flasks, respectively adding triethanolamine, water, hydroxylamine hydrochloride, a potassium hydroxide, several drops of magnesium sulfate and a proper amount of a calcein indicator into one group in sequence, and titrating by EDTA until fluorescent green disappears; respectively adding triethanolamine, water, hydroxylamine hydrochloride, an ammonia-ammonia chloride buffering solution and an eriochrome black T indicator, and titrating by EDTA until amaranth is turned into blue, and obtaining the content of magnesium.
Description
Technical field
The invention belongs to ferroalloy analysis field, relate to the method for continuously measuring of content of calcium and magnesium in a kind of volumetric determination Si―Si bond.
Background technology
Deoxygenation of liquid steel is requisite process procedure in steelmaking process, and wherein the selection of deoxidizer is most important.From the history of deoxidant for steelmaking, the initial fine aluminium (generally using aluminium cake, Al content >95%) used, due to light specific gravity (2.79gPcm
3), aluminium cake not easily gos deep into molten steel inside, thus limits the effective rate of utilization of aluminium element.The ferro-silico aluminium that rear employing is made up of Si, Al Was Used replaces aluminium cake, therefore heavily increases (about 4.3gPcm
3), the effective rate of utilization of Al element is significantly improved, the consumption also corresponding reduction of deoxidant for steelmaking.In recent years, along with steel are by the conversion of the seller to buyer's market, enterprise is forced more to focus on improving the inherent quality of steel.Double deoxidizer is strong because having deoxidizing capacity, can obviously improve the advantages such as molten steel degree of purity, naturally the common concern of numerous research institution and iron and steel enterprise is subject to, become the focus of recent deoxidizer field Study and Development, wherein especially to contain alkaline earth element Ba, the double deoxidizer research of Ca is the most active, the selection of deoxidizer, aluminium is as traditional deoxidant for steelmaking, strong and the aluminium because of aluminium and oxygen affinity, the characteristic of dissolving each other completely between iron, this also determines aluminium must status more difficult change in for a long time of ingredient as steel-making end-deoxidizer, but because aluminium adds easy formation high-melting-point deoxidation products in steel, molten steel flow is deteriorated, the castability of molten steel can be had a strong impact on, thus the direct motion that continuous casting is produced is constituted a threat to, therefore during deoxidation in steel making, the addition of aluminium is restricted.
Research shows, effectively degenerative treatments can be carried out to the high-melting-point snotter that deoxidation produces containing introducing strong deoxidant element Ca in the deoxidizer of aluminium, thus significantly improve the mobility of aluminium deoxidation molten steel, but because Ca self still also exists as in steel, solubleness is low, light specific gravity, the weakness such as vapor pressure is high, how to improve its effective rate of utilization and become the problem must considered when determining that deoxidizer forms, research shows, Ba element itself is not only have than great, the strong deoxidizer that steam forces down, and dissolve each other completely with Ca, and the vapor pressure of Ca is obviously reduced with the increase of its content, therefore the low aluminium composite deoxidant of high barium of development and application calcic become ferroalloy producer and steel mill common faced by problem, represent the developing direction of deoxidant for steelmaking from now on.
Si-Al-Ba-Ca is best deoxidizer, desulfurizing agent in barium system alloy, and the oxygen in steel is dropped to minimum, the complex oxide of the calcic simultaneously formed, barium, silicon, aluminium easily floats from molten steel, pure molten steel, improves tough and the processability of steel.Si-Al-Ba-Ca is high efficiency deoxidiser is steel-making auxiliary material, it is adapted to the deoxidation of multiple steel-making form, especially pneumatic steelmaking deoxidation is applicable to, there is very strong deoxidation, desulfurized effect, MOLTEN STEEL FLOW performance can be improved well, solve nozzle clogging problem, reduce gas in steel, reduction molten steel is mingled with, the Accurate Determining therefore carrying out content of calcium and magnesium in Si―Si bond is significant.
The method large enterprise of mensuration calcium, magnesium adopts large-scale instrument analysis mostly, but cost is high, and for small business, chemical analysis method embodies its advantage more, namely convenient, fast.Chemical analysis calcium magnesium major part separately measures, and waste reagent, cost is high.The mensuration of calcium magnesium is generally separated interference element with ammoniacal liquor, operates more loaded down with trivial details, time-consuming.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of more fast, measure the method for content of calcium and magnesium in Si―Si bond accurately and efficiently.
For reaching above-mentioned purpose, the method for continuously measuring of content of calcium and magnesium in a kind of Si―Si bond of the present invention, comprises the following steps:
The Si―Si bond sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor respectively afterwards, low temp. electric hot plate dissolves, add perchloric acid smoked afterwards, cigarette emits only, and sample is withered adds hydrochloric acid heating for dissolving salt, and test solution is transferred in Large Copacity bottle and is diluted to scale constant volume;
From the sample solution after constant volume and blank solution, divide and get the quantitative solution of equivalent two parts respectively in beaker, a sample and blank solution add triethanolamine, water, oxammonium hydrochloride respectively successively, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, and being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, and meter lower volume is respectively V
caand V
01, obtaining calcium content is: W
ca%=C (V
ca-V
0) M
ca100/mK × 100;
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
ca: sample consumes the volume of EDTA standard solution, mL;
V
01: the blank volume consuming EDTA standard solution, mL;
Another increment product and blank solution add and add triethanolamine, water respectively successively, add oxammonium hydrochloride, ammonification-ammonium chloride buffer solution keeps pH=10, add chromium black T indicator appropriate, being titrated to aubergine with the EDTA standard solution that concentration is C, to become blueness be terminal, and meter lower volume is respectively V
mg+Caand V
02, obtaining content of magnesium is W
mg%=C (V
mg+Ca-V
ca-(V
02-V
01) M
mg100/mK × 1000;
In formula: M
mg: magnesian molal weight, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
mg+Ca: calcium magnesium resultant consume the volume of EDTA standard solution, mL;
V
02: the blank volume consuming EDTA standard solution during titration calcium magnesium resultant, mL.
Wherein said nitric acid and described hydrofluorite volumetric usage are 1:1, and concentration is respectively 67% and 40%.
Wherein on low temp. electric hot plate at 100 DEG C dissolved samples.
Wherein said perchloric acid concentration is 70%.
Wherein said concentration of hydrochloric acid is 65%.
Wherein said triethanolamine concentrations is 12%.
Wherein said concentration of potassium hydroxide is 20%.
Wherein said magnesium sulfate concentration is 0.5%.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) fast, efficiently, low cost: the method substantially reduces operating process, has saved medicine, has reduced testing cost, improve production efficiency;
2) accurately, stable: the mensuration of this method calcium, magnesium adopt triethanolamine to shelter interference element and ammoniacal liquor to be separated interference element measurement result for twice the same.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary: adopt nitric acid (67%)-hydrofluorite (40%) dissolved samples in vinyon beaker, add perchloric acid (70%) and smolder, cigarette emits only, and one lights a cigarette cannot see, and test solution dries up.Add 10mL hydrochloric acid (65%), heating for dissolving salt.Test solution is transferred in 250mL volumetric flask, be diluted to scale constant volume.Divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%, keep pH to be not less than 12), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal; Another part adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add chromium black T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal.
2. reagent:
2.1 nitric acid (67%)
2.2 hydrofluorite (40%)
2.3 perchloric acid (70%)
2.4 hydrochloric acid (65%)
2.5 oxammonium hydrochlorides (solid)
2.6 triethanolamines (12%)
2.7 potassium hydroxide solutions (20%)
2.8 calcein indicator: 1g calcein and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
2.9EDTA standard solution C (EDTA)=0.01783mol/L
2.10 ammonia-ammonium chloride buffer solution (pH=10): 67g ammonium chloride is dissolved in 200mL water, adds 570mL strong aqua, is diluted to 1000mL. with water
2.11 chromium black T indicators: 1g eriochrome black T and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
3. sampling and sample preparation: get sample preparation standard according to ferroalloy and carry out sample and produce.
4. sample weighting amount: take sample 0.2500g
5. analytical procedure:
Take sample m0.2500g in polytetrafluoroethylene beaker, add 10mL nitric acid (67%), add 10mL hydrofluorite (40%), dissolved samples on electric hot plate, after sample major part is dissolved, adds 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one and lights a cigarette, take off, add hydrochloric acid (65%) 10mL, heating for dissolving salt, transfers to test solution in 250mL volumetric flask, is diluted to scale fixed molten.From 250mL volumetric flask, divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), adds 50mL water, adds oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%, pH is kept to be not less than 12), calcein indicator is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume is V
ca.Another part adds 50mL triethanolamine (12%), adds 50mL water, adds oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add chromium black T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal, and meter lower volume is V
mg+Ca.
Blank assay
In polytetrafluoroethylene beaker, add 10mL nitric acid (67%), add 10mL hydrofluorite (40%), dissolved samples on electric hot plate, after sample major part is dissolved, adds 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one and lights a cigarette, take off, add hydrochloric acid (65%) 10mL, heating for dissolving salt, transfers to test solution in 250mL volumetric flask, is diluted to scale fixed molten.Divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%, keep pH to be not less than 12), calcein indicator is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume is V01.Another part adds 50mL triethanolamine (12%), adds 50mL water, adds oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add chromium black T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal, and meter lower volume is V
02.
6. Analysis result calculation:
W
Ca％＝C(V
Ca-V
01)M
Ca100/mK×1000
In formula: M
ca: the molal weight (g/mol) of calcium
M: sample mass (g)
K: sample divides liquor ratio (50/250=1/5), the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution (mol/L)
V
ca: in sample, calcium consumes the volume (mL) of EDTA standard solution
V
01: the blank volume (mL) consuming EDTA standard solution during titration calcium
W
Mg％＝C(V
Mg+Ca-V
Ca-(V
02-V
01)M
Mg100/mK×1000
In formula: M
mg: magnesian molal weight (g/mol)
M: sample mass (g)
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution (mol/L)
V
mg+Ca: calcium magnesium resultant consume the volume (mL) of EDTA standard solution
V
02: the blank volume (mL) consuming EDTA standard solution during titration calcium magnesium resultant
7. standard specimen analysis of control: because Si-Ca-Ba-Mg does not have suitable standard specimen therefore to adopt silicon aluminum calcium barium alloy standard specimen
The comparison of calcium:
As can be seen from the above table: the data that calcium content gained in data and the ammoniacal liquor twice separation determination silicon aluminum calcium barium alloy measuring calcium content gained in silicon aluminum calcium barium alloy directly sheltered by use triethanolamine are the same, and accurately, and operating process is short, fast, efficient.
Precision:
As can be seen from the above table: precision is fine.
8. conclusion:
The content of calcium and magnesium in Si―Si bond can be determined continuously accurately by the inventive method.Substantially reduce the running time, reduce energy consumption.Make determination data accurately and reliably, application obtains good effect aborning.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (8)
1. the method for continuously measuring of content of calcium and magnesium in Si―Si bond, is characterized in that comprising the following steps:
The Si―Si bond sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor respectively afterwards, low temp. electric hot plate dissolves, add perchloric acid smoked afterwards, cigarette emits only, and sample is withered adds hydrochloric acid heating for dissolving salt, and test solution is transferred in Large Copacity bottle and is diluted to scale constant volume;
From the sample solution after constant volume and blank solution, divide and get the quantitative solution of equivalent two parts respectively in beaker, a sample and blank solution add triethanolamine, water, oxammonium hydrochloride respectively successively, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, and being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, and meter lower volume is respectively V
caand V
01, obtaining calcium content is: W
ca%=C (V
ca-V
0) M
ca100/mK × 100;
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
ca: sample consumes the volume of EDTA standard solution, mL;
V
01: the blank volume consuming EDTA standard solution, mL;
Another increment product and blank solution add and add triethanolamine, water respectively successively, add oxammonium hydrochloride, ammonification-ammonium chloride buffer solution keeps pH=10, add chromium black T indicator appropriate, being titrated to aubergine with the EDTA standard solution that concentration is C, to become blueness be terminal, and meter lower volume is respectively V
mg+Caand V
02, obtaining content of magnesium is W
mg%=C (V
mg+Ca-V
ca-(V
02-V
01) M
mg100/mK × 1000;
In formula: M
mg: magnesian molal weight, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
mg+Ca: calcium magnesium resultant consume the volume of EDTA standard solution, mL;
V
02: the blank volume consuming EDTA standard solution during titration calcium magnesium resultant, mL.
2. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described nitric acid and described hydrofluorite volumetric usage are 1:1, and concentration is respectively 67% and 40%.
3. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: on low temp. electric hot plate at 100 DEG C dissolved samples.
4. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described perchloric acid concentration is 70%.
5. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described concentration of hydrochloric acid is 65%.
6. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described triethanolamine concentrations is 12%.
7. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described concentration of potassium hydroxide is 20%.
8. the method for continuously measuring of content of calcium and magnesium in Si―Si bond according to claim 1, is characterized in that: described magnesium sulfate concentration is 0.5%.
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| CN113322054A (en) * | 2020-02-28 | 2021-08-31 | 中国石油化工股份有限公司 | Magnesium alloy dissolving agent |
| CN113322054B (en) * | 2020-02-28 | 2022-07-22 | 中国石油化工股份有限公司 | Magnesium alloy dissolving agent |
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