CN101303313B - Method for measuring triethanolamine in aluminum alloy basification milling solution - Google Patents

Method for measuring triethanolamine in aluminum alloy basification milling solution Download PDF

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Publication number
CN101303313B
CN101303313B CN2008101327231A CN200810132723A CN101303313B CN 101303313 B CN101303313 B CN 101303313B CN 2008101327231 A CN2008101327231 A CN 2008101327231A CN 200810132723 A CN200810132723 A CN 200810132723A CN 101303313 B CN101303313 B CN 101303313B
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triethanolamine
aluminum alloy
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alloy basification
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CN101303313A (en
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王振林
于四龙
杨红
孙浩
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Harbin Aircraft Industry Group Co Ltd
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Harbin Aircraft Industry Group Co Ltd
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Abstract

The invention relates to a measurement method for triethanolamine in an alkaline solution of aluminum mill, belonging to the field of chemical analysis, characterized by comprising measurement steps of preparing reagents, drawing work curves, preparing the alkaline solution of aluminum mill to be measured, and measuring triethanolamine content. The invention greatly improves measurement precision of triethanolamine content in the alkaline solution of aluminum mill and quality of the chemical milling.

Description

The assay method of triethanolamine in the aluminum alloy basification milling solution
Technical field
The invention belongs to chemical analysis technology, relate to the assay method of triethanolamine in a kind of aluminum alloy basification milling solution.
Background technology
Chemistry milling is in the industry-wide a kind of important aluminium alloy job operation of Aeronautics and Astronautics.Milling technology can replace some machining, remove excess metal from the piece surface corrosion, to change its size and to alleviate its weight, in addition, when machining can not reach and milling can satisfy the Element Design requirement time, also this kind processes can be adopted, all milling technology can be adopted as hyperboloid, large-area thin plate spare and other complex parts.The quality of part chemistry milling depends on the quality of chemistry milling solution, but, analytical approach for the chemistry milling solution composition does not still have unified standard at present, the present major control NaOH of each enterprise, two indexs of aluminium, and the content of triethanolamine is not measured, generally in suitable scope, this method error is very big, can not guarantee the crudy of chemistry milling for the content of determining this material according to the surfaceness situation of test piece.
Summary of the invention
The objective of the invention is: propose a kind ofly can accurately measure triethanolamine Determination on content method in the aluminum alloy basification milling solution, measure precision and milling crudy to improve.
Technical scheme of the present invention is: the assay method of triethanolamine in the aluminum alloy basification milling solution is characterized in that the step of mensuration is as follows:
1, reagent is prepared;
1.1, ammonium fluoride solution: concentration is 100g/L;
1.2, sodium hydroxide solution: concentration is 50g/L;
1.3, ammoniacal liquor: density is 0.89g/mL;
1.4, Ammonium Vanadate Solution: take by weighing the 22.96g ammonium vanadate and be dissolved in the distilled water, add 15.7g NaOH again, to 1000mL, it is standby to filter the back with distilled water diluting for dissolving back;
1.5, oxammonium hydrochloride solution: concentration is 100g/L;
1.6, the triethanolamine standard solution: concentration is 10mg/mL; Compound method is: take by weighing the 5.0000g triethanolamine and place volumetric flask, adding distil water is diluted to 500mL, and it is standby to shake up the back;
1.7, do not add the aluminum alloy basification milling solution of triethanolamine: the aluminum alloy basification milling solution that does not add triethanolamine according to the formulated of navigation mark regulation;
2, drawing curve;
2.1, preparation has the aluminum alloy basification milling solution of known content triethanolamine; Draw the aluminum alloy basification milling solution that 1.00mL does not add triethanolamine respectively, place 7 250mL conical flasks, add triethanolamine standard solution 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL respectively with microburette, obtain having the aluminum alloy basification milling solution of known content triethanolamine;
2.2, measure the absorbance of aluminum alloy basification milling solution with known content triethanolamine; With 1 cm cuvette, be reference solution with distilled water, use spectrophotometer to measure absorbance in 510nm wavelength place;
2.3, the drawing curve; Content with triethanolamine is horizontal ordinate, is ordinate with the absorbance, and the drawing curve connects with straight line between 2;
3, prepare determined aluminum alloy basification milling solution; From the milling groove, accurately pipette the filtered aluminum alloy basification milling solution of 1.00mL in conical flask, add 50mL distilled water and 8mL ammonium fluoride solution, transfer to pH value of solution=11 ± 0.2 with sodium hydroxide solution, shake up behind the adding 5mL ammoniacal liquor, add 6.00mL Ammonium Vanadate Solution and 2mL oxammonium hydrochloride solution again, be heated to boiling 60 ± 10 seconds, when solution presents redness, stop heating, be cooled to room temperature, move in the 100mL volumetric flask with flowing water,, shake up to scale with distilled water diluting;
4, measure the content of triethanolamine; Using the 1cm cuvette, is reference solution with distilled water, uses spectrophotometer to measure absorbance in 510nm wavelength place, checks in the content of triethanolamine the determined aluminum alloy basification milling solution from working curve.
Advantage of the present invention is: improved the survey precision and the milling crudy of triethanolamine content in the aluminum alloy basification milling solution greatly.
Embodiment
Below the present invention is described in further details.The assay method of triethanolamine is characterized in that in the aluminum alloy basification milling solution, and the step of mensuration is as follows:
1, reagent is prepared;
1.1, ammonium fluoride solution: concentration is 100g/L;
1.2, sodium hydroxide solution: concentration is 50g/L;
1.3, ammoniacal liquor: density is 0.89g/mL;
1.4, Ammonium Vanadate Solution: take by weighing the 22.96g ammonium vanadate and be dissolved in the distilled water, add 15.7g NaOH again, to 1000mL, it is standby to filter the back with distilled water diluting for dissolving back;
1.5, oxammonium hydrochloride solution: concentration is 100g/L;
1.6, the triethanolamine standard solution: concentration is 10mg/mL; Compound method is: take by weighing the 5.0000g triethanolamine and place volumetric flask, adding distil water is diluted to 500mL, and it is standby to shake up the back;
1.7, do not add the aluminum alloy basification milling solution of triethanolamine: the aluminum alloy basification milling solution that does not add triethanolamine according to the formulated of navigation mark regulation;
2, drawing curve;
2.1, preparation has the aluminum alloy basification milling solution of known content triethanolamine; Draw the aluminum alloy basification milling solution that 1.00mL does not add triethanolamine respectively, place 7 250mL conical flasks, add triethanolamine standard solution 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL respectively with microburette, obtain having the aluminum alloy basification milling solution of known content triethanolamine;
2.2, measure the absorbance of aluminum alloy basification milling solution with known content triethanolamine; Using the 1cm cuvette, is reference solution with distilled water, uses spectrophotometer to measure absorbance in 510nm wavelength place;
2.3, the drawing curve; Content with triethanolamine is horizontal ordinate, is ordinate with the absorbance, and the drawing curve connects with straight line between 2;
3, prepare determined aluminum alloy basification milling solution; From the milling groove, accurately pipette the filtered aluminum alloy basification milling solution of 1.00mL in conical flask, add 50mL distilled water and 8mL ammonium fluoride solution, transfer to pH value of solution=11 ± 0.2 with sodium hydroxide solution, shake up behind the adding 5mL ammoniacal liquor, add 6.00mL Ammonium Vanadate Solution and 2mL oxammonium hydrochloride solution again, be heated to boiling 60 ± 10 seconds, when solution presents redness, stop heating, be cooled to room temperature, move in the 100mL volumetric flask with flowing water,, shake up to scale with distilled water diluting;
4, measure the content of triethanolamine; Using the 1cm cuvette, is reference solution with distilled water, uses spectrophotometer to measure absorbance in 510nm wavelength place, checks in the content of triethanolamine the determined aluminum alloy basification milling solution from working curve.
Embodiment.
Prepare the aluminium alloying groove milling liquid that contains triethanolamine 44.0g/L, 45.0g/L, 50.0g/L respectively and carry out demonstration test, the test figure that obtains sees the following form 1.
The determination test method validation test figure of table 1 triethanolamine
The sample title Standard triethanolamine content (g/L) Sampling amount (mL) Absorbance The triethanolamine content of measuring (g/L) The recovery (%)
Aluminum alloy basification milling solution 44.0 1.00 0.470 42.7 97.0
Aluminum alloy basification milling solution 45.0 1.00 0.480 43.5 96.7
Aluminum alloy basification milling solution 50.0 1.00 0.530 48.2 96.4
Find out that by table 1 recovery of measurement result is all more than 95%.

Claims (1)

1. the assay method of triethanolamine in the aluminum alloy basification milling solution is characterized in that, the step of mensuration is as follows:
1.1, reagent prepares;
1.1.1, ammonium fluoride solution: concentration is 100g/L;
1.1.2, sodium hydroxide solution: concentration is 50g/L;
1.1.3, ammoniacal liquor: density is 0.89g/mL;
1.1.4, Ammonium Vanadate Solution: take by weighing the 22.96g ammonium vanadate and be dissolved in the distilled water, add 15.7g NaOH again, to 1000mL, it is standby to filter the back with distilled water diluting for dissolving back;
1.1.5, oxammonium hydrochloride solution: concentration is 100g/L;
1.1.6, the triethanolamine standard solution: concentration is 10mg/mL; Compound method is: take by weighing the 5.0000g triethanolamine and place volumetric flask, adding distil water is diluted to 500mL, and it is standby to shake up the back;
1.1.7, do not add the aluminum alloy basification milling solution of triethanolamine: the aluminum alloy basification milling solution that does not add triethanolamine according to the formulated of navigation mark regulation;
1.2, the drawing curve;
1.2.1, preparation has the aluminum alloy basification milling solution of known content triethanolamine; Draw the aluminum alloy basification milling solution that 1.00mL does not add triethanolamine respectively, place 7 250mL conical flasks, add triethanolamine standard solution 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL respectively with microburette, obtain having the aluminum alloy basification milling solution of known content triethanolamine;
1.2.2, measure the absorbance of aluminum alloy basification milling solution with known content triethanolamine; Using the 1cm cuvette, is reference solution with distilled water, uses spectrophotometer to measure absorbance in 510nm wavelength place;
1.2.3, the drawing curve; Content with triethanolamine is horizontal ordinate, is ordinate with the absorbance, and the drawing curve connects with straight line between 2;
1.3, prepare determined aluminum alloy basification milling solution; From the milling groove, accurately pipette the filtered aluminum alloy basification milling solution of 1.00mL in conical flask, add 50mL distilled water and 8mL ammonium fluoride solution, transfer to pH value of solution=11 ± 0.2 with sodium hydroxide solution, shake up behind the adding 5mL ammoniacal liquor, add 6.00mL Ammonium Vanadate Solution and 2mL oxammonium hydrochloride solution again, be heated to boiling 60 ± 10 seconds, when solution presents redness, stop heating, be cooled to room temperature, move in the 100mL volumetric flask with flowing water,, shake up to scale with distilled water diluting;
1.4, measure the content of triethanolamine; Using the 1cm cuvette, is reference solution with distilled water, uses spectrophotometer to measure absorbance in 510nm wavelength place, checks in the content of triethanolamine the determined aluminum alloy basification milling solution from working curve.
CN2008101327231A 2008-07-11 2008-07-11 Method for measuring triethanolamine in aluminum alloy basification milling solution Expired - Fee Related CN101303313B (en)

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CN102330088B (en) * 2011-11-02 2013-07-17 沈阳飞机工业(集团)有限公司 Chemical milling solution for aluminum-lithium alloy
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1239563A1 (en) * 1984-08-15 1986-06-23 Научно-исследовательский и проектный институт по обогащению и агломерации руд черных металлов "Механобрчермет" Method of determining triethanolamine in industrial effluent
CN101122025A (en) * 2007-08-09 2008-02-13 成都飞机工业(集团)有限责任公司 Titanium alloying milling solution and milling technique used for the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1239563A1 (en) * 1984-08-15 1986-06-23 Научно-исследовательский и проектный институт по обогащению и агломерации руд черных металлов "Механобрчермет" Method of determining triethanolamine in industrial effluent
CN101122025A (en) * 2007-08-09 2008-02-13 成都飞机工业(集团)有限责任公司 Titanium alloying milling solution and milling technique used for the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
徐功骅,等.铝材化铣成分分析技术.《航空工程与维修》.1996,(第9期),
徐功骅等.铝材化铣成分分析技术.《航空工程与维修》.1996,(第9期), *

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