CN103604767B - The assay method of cobalt content in cutting oil - Google Patents
The assay method of cobalt content in cutting oil Download PDFInfo
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- CN103604767B CN103604767B CN201310611073.XA CN201310611073A CN103604767B CN 103604767 B CN103604767 B CN 103604767B CN 201310611073 A CN201310611073 A CN 201310611073A CN 103604767 B CN103604767 B CN 103604767B
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Abstract
The invention provides the assay method of cobalt content in a kind of cutting oil, comprise the step of cutting oil sample being carried out to ashing, acid-soluble, constant volume, mensuration absorbance; Cineration step is for to be warming up to 450～500 DEG C by heating schedule by cutting oil, and heating schedule is to heat up 50～80 DEG C for every 20～30 minutes. The method just can obtain cobalt content in cutting oil by heating, ashing, mensuration absorbance step, and simple to operate, result is accurate. Be used in cutter and repair in monitor procedure, can find that in cutting oil, cobalt content exceeds standard, change in time cutting oil, slow down tool wear, annual cutter consumption reduces 10%, and cutter repair rate has improved 15%.
Description
Technical field
The present invention relates to technical Analysis chemical field, in particular to the assay method of cobalt content in a kind of cutting oil.
Background technology
In machining, cutter is a kind of conventional workpiece. Cutter is usually used in cutting all kinds of parts, needs cutting oil in use procedureBring into play the effects such as lubricated, cooling. After cutter rust after use, need to make it again sharp keen through repairing, polished in repairingIn journey, also need cutting oil to be lubricated cooling cutter. In above-mentioned use procedure, the cobalt element in cutter can enter cutting oil. CuttingOil is after Reusability, and wherein cobalt content constantly rises, and part cobalt can be separated out with the form of particle. The cobalt granule rigidity of separating out is large,Cause the further wearing and tearing of cutter in working angles.
Summary of the invention
The present invention aims to provide the assay method of cobalt content in a kind of cutting oil, lacks cobalt content in cutting oil to solve prior artThe problem of assay method.
To achieve these goals, according to the assay method that the invention provides cobalt content in a kind of cutting oil, comprise cutting oilSample carries out the step of ashing, acid-soluble, constant volume, mensuration absorbance; Cineration step is for to be warming up to cutting oil by heating schedule450～500 DEG C, heating schedule is to heat up 50～80 DEG C for every 20～30 minutes.
Further, acid-soluble for adding in chloroazotic acid, red fuming nitric acid (RFNA) or concentrated hydrochloric acid and heating by residue obtained after ashing.
Further, measure the calibration curve that also comprises the standard liquid of measuring cobalt in absorbance step, comprise the following steps:
1) mass fraction is greater than to 99.99% the acid-soluble solution of cobalt, being settled to concentration is the to be determined of 0.01000～0.5000mg/100mlStandard cobalt liquor;
2) get standard cobalt liquor 0.05ml to be determined, 0.10ml, 0.15ml, 0.20ml, 0.25ml, 0.30ml, 0.35ml respectivelyConstant volume, obtains standard liquid;
3) absorbance of bioassay standard solution respectively, and taking gained absorbance as ordinate and concentration of standard solution paint as abscissaCalibration curve processed.
Technique effect of the present invention is:
Method provided by the invention just can obtain cobalt content in cutting oil by heating, ashing, mensuration absorbance step, operation letterSingle, result is accurate. Be used in cutter repair process, can find that in time in cutting oil, cobalt content exceeds standard, change cutting oil, subtractSlow tool wear, annual cutter consumption reduces 10%. Cutter repair rate has improved 15%.
Except object described above, feature and advantage, the present invention also has other object, feature and advantage. BelowWith reference to embodiment, the present invention is further detailed explanation.
Detailed description of the invention
It should be noted that, in the situation that not conflicting, the feature in embodiment and embodiment in the application can combine mutually.Describe the present invention in detail below in conjunction with embodiment.
Method energy Quick Measuring provided by the invention obtains cobalt content in cutting oil, easy and simple to handle, reliable results, and the used time only needs 6 hours.
Method provided by the invention comprises carries out ashing, cooling, acid-soluble, cooling, constant volume, mensuration absorbance to cutting oil sampleStep. Cutting oil is mixed by multiple grease. In cutting oil after use, dissolved in Determination of multiple metal elements, as iron, nickel,Chromium, cobalt etc. These elements form mixed system mainly with small particle form and grease. These metallic particles are by a large amount of cutting oilsSurround, cause great difficulty to the mensuration of cobalt, there is no at present analytical method, so metallic particles is the party with separating of cutting oilThe key of method. By ashing, the organic principle in cutting oil sample is removed. Ashing temperature is 450～500 DEG C. In order to prevent heating upThe boiling of cutting oil sample, burning, vaporization in process, cause cobalt loss, makes detected value on the low side, and programming rate can not be too fast, shouldAshing again after first making cutting oil solidify, heats up by the program of 50～80 DEG C of 20～30min intensifications. Most of material in cutting oilFor grease, macromolecule grease at high temperature mostly occur carbonization produce carbon, the carbon of high temperature is combined with CO with airborne oxygen2FormLeave. So, the most of organic principle in cutting oil sample is removed. The metallic element of free state stays with the form of residue.The heating schedule that adopts 50 DEG C of 30min intensifications, the required heating-up time is the shortest, and impurity volatilization is the most thorough. After ashing, cooling gained is residualSlag is proceeded following chemical treatment.
Acid-soluble step is for dissolving residue obtained ashing with 10ml chloroazotic acid, red fuming nitric acid (RFNA) or concentrated hydrochloric acid. Main in residue after ashingContain cobalt, residue is dissolved in after chloroazotic acid, and cobalt element exists in solution with ionic species. In order to promote residue to dissolve, acid-solubleIn step, the solution that is dissolved with residue is heated to 100～150 DEG C. Treat that residue dissolves completely, is cooled to room temperature.
The means of measuring cobalt have: atomic absorption spectrophotometry, ICP method, colorimetric method, EDTA volumetric method, this patent is selected formerSub-absorptiometry is measured cobalt, atomic absorption spectrophotometry is used compared with other method equipment operating is simple,Low price, highly sensitive to cobalt, measure cobalt by atomic absorption spectrophotometry, and in cutting oil, iron, nickel, chromium are to itNoiseless, so trace cobalt in the most applicable mensuration cutting oil of atomic absorption spectrophotometry. To using and steam through acid-soluble solution gained solutionHeating up in a steamer water is settled to 100ml and obtains cobalt liquor to be measured. According to cobalt liquor to be measured at the absorbance at 240.7nm wavelength place from cobalt standardIn curve, read for cobalt concentration. If cobalt liquor excessive concentration to be measured cannot obtain in this calibration curve, molten to cobalt to be measuredLiquid carries out dilution process, and concrete extension rate is determined according to solution concentration. Again measure the cobalt liquor absorbance to be measured after dilutionValue, and from calibration curve, obtain corresponding cobalt concentration. Absorbance is for measuring with atomic absorption spectrophotometer.
Bioassay standard curve map, can record according to the assay method of conventional analysis chemistry Plays curve. Standard curve determination methodComprise the following steps:
1) take the cobalt that 0.01000～0.5000g mass fraction is greater than 99.99%, add 10ml nitric acid, dissolved cobalt is boiled in heatingObtain cobalt liquor;
2) cobalt liquor is settled to 100ml, shakes up and obtain standard cobalt liquor to be determined, get respectively 0.05ml, 0.10ml, 0.15ml,0.20ml, 0.25ml, this constant volume solution of 0.30ml, 0.35ml, be settled to respectively 100ml again and obtain standard liquid;
3) above-mentioned standard liquid is added to 5ml nitric acid respectively
4) measure each standard liquid absorbance in 240.7nm wavelength place, taking concentration of standard solution as abscissa, each standard liquidCorresponding absorbance is ordinate, drawing standard curve.
Concrete standard cobalt liquor concentration used is 0.01～0.5mg/ml. By the absorption photometric value substitution standard song of measured solution to be measuredIn line, obtain corresponding cobalt liquor concentration. This cobalt liquor concentration is exactly the concentration of cobalt in solution to be measured. Thereby extrapolate cutting oilThe amount of contained cobalt in sample. Again cobalt content standard in the amount of gained cobalt and cutting oil is compared. If the amount of gained cobalt higher thanCobalt content standard needs to change cutting oil, avoids the damage to cutter of cobalt too much in cutting oil. The mark that adopts said method to makeThe directrix curve degree of accuracy is high, and the used time is few.
Embodiment
In following examples, each material used and instrument are commercially available.
The drafting of cobalt calibration curve: the standard liquid of preparation cobalt, concentration 0.01～0.5mg/100ml. Record each concentration standard cobalt moltenLiquid is in the absorbance at 240.7nm place, and taking cobalt concentration as abscissa, absorbance is that ordinate is drawn cobalt canonical plotting.
Embodiment 1
A takes the cutting oil sample of 0.5000g in 100ml porcelain crucible, within every 30 minutes, heats up 50 DEG C, is progressively warmed up to 500DEG C, ashing cutting oil, obtains residue.
B trub, adds 10ml chloroazotic acid by residue and obtains wang aqueous solution, wang aqueous solution is heated to 100～150 DEG C with electric furnace,Treat that residue dissolves completely, is cooled to room temperature. With 100ml volumetric flask constant volume. With atomic absorption spectrophotometer at 240.7nm rippleStrong point is measured the absorbance of gained solution.
C, according to surveyed absorbance, inquires about cobalt concentration from cobalt canonical plotting. When cannot be when calibration curve obtains cobalt concentration,To 2 times of cobalt liquor dilutions after constant volume. Again measure the absorbance of cobalt liquor after dilution, and from cobalt calibration curve, check in cobaltConcentration, and extrapolate the content of cobalt in cutting oil sample.
Embodiment 2
A takes the cutting oil sample of 0.5000g in 100ml porcelain crucible, within every 20 minutes, heats up 80 DEG C, is progressively warmed up to 450DEG C, ashing cutting oil, obtains residue.
B trub, adds 10ml chloroazotic acid by residue and obtains wang aqueous solution, wang aqueous solution is heated to 100～150 DEG C with electric furnace,Treat that residue dissolves completely, is cooled to room temperature. With 100ml volumetric flask constant volume. With atomic absorption spectrophotometer at 240.7nm rippleStrong point is measured the absorbance of gained solution.
C, according to surveyed absorbance, inquires about cobalt concentration from cobalt canonical plotting. When cannot be when calibration curve obtains cobalt concentration,To 2 times of cobalt liquor dilutions after constant volume. Again measure the absorbance of cobalt liquor after dilution, and from cobalt calibration curve, check in cobaltConcentration, and extrapolate the content of cobalt in cutting oil sample.
Embodiment 3
A takes the cutting oil sample of 0.5000g in 10Oml porcelain crucible, within every 23 minutes, heats up 70 DEG C, is progressively warmed up to 500DEG C, ashing cutting oil, obtains residue.
B trub, adds 10ml chloroazotic acid by residue and obtains wang aqueous solution, wang aqueous solution is heated to 100～150 DEG C with electric furnace,Treat that residue dissolves completely, is cooled to room temperature. With 100ml volumetric flask constant volume. With atomic absorption spectrophotometer at 240.7nm rippleStrong point is measured the absorbance of gained solution.
C, according to surveyed absorbance, inquires about cobalt concentration from cobalt canonical plotting. When cannot be when calibration curve obtains cobalt concentration,To 2 times of cobalt liquor dilutions after constant volume. Again measure the absorbance of cobalt liquor after dilution, and from cobalt calibration curve, check in cobaltConcentration, and extrapolate the content of cobalt in cutting oil sample.
Comparative example
Do not adopt the method that the application provides to detect cobalt content in cutting oil.
Cutter uses the cutting oil after 1 month, it being used to carry out cobalt content detection.
By the content of cobalt in monitoring cutting oil, change in time cutting oil, slow down the wearing and tearing of cutter, embodiment and comparative example phaseReduce 10% than annual cutter use amount. Cutter repair in the quality control of the cutting oil that uses, by the monitoring to cobalt, cutterTool repair rate improves 15%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art, the present invention can have various modifications and variations. Within the spirit and principles in the present invention all, any amendment of doing, etc.With replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (2)
1. an assay method for cobalt content in cutting oil, comprises that cutting oil to be determined is carried out to ashing, acid-soluble, constant volume, mensuration to be inhaledThe step of luminosity, is characterized in that, described cineration step is for to be warming up to 450～500 DEG C by heating schedule by described cutting oil,Described heating schedule is to heat up 50～80 DEG C for every 20～30 minutes;
Described acid-soluble for adding in chloroazotic acid, red fuming nitric acid (RFNA) or concentrated hydrochloric acid and heating by residue obtained after described ashing, in acid-soluble stepIn rapid, the solution that is dissolved with residue is heated to 100～150 DEG C.
2. method according to claim 1, is characterized in that, in described mensuration absorbance step, also comprises the standard of measuring cobaltThe calibration curve of solution, comprises the following steps:
1) mass fraction is greater than to 99.99% the acid-soluble solution of cobalt, being settled to concentration is treating of 0.01000～0.5000mg/100mlBioassay standard cobalt liquor;
2) get described standard cobalt liquor 0.05ml to be determined, 0.10ml, 0.15ml, 0.20ml, 0.25ml, 0.30ml, 0.35mlConstant volume, obtains standard liquid respectively;
3) measure respectively the absorbance of described standard liquid, and taking gained absorbance as ordinate and concentration of standard solution asAbscissa drawing standard curve.
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| CN107525796A (en) * | 2016-06-22 | 2017-12-29 | 上海宝钢工业技术服务有限公司 | The assay method of iron content in emulsion |
| CN112198186A (en) * | 2020-07-28 | 2021-01-08 | 重庆安美新材料有限公司 | Method for testing high-temperature stability of cutting fluid |
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