CN101165470A - Surface organic compound concentration measuring method - Google Patents
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Abstract
Relationship formulas A/D>=2 and B>= (A+D) should be satisfied, wherein, A is the diameter of the area irradiated by the infrared, and D is the outer diameter of the cylindraceous or the circular column-shaped object to be measured, and B is the set width when a plurality of objects to be measured are arranged in parallel in the area irradiated by the infrared. the cylindraceous or the circular column-shaped objects to be measured are arranged in the area irradiated by the infrared and are irradiated by the infrared, and the absorbency of the dispersion reflected light of the object to be measured to the infrared with a special wavelength will be measured. Thus, the attachment amounts of oil coated on the object can be measured simply in high-precision by using said measuring method without being influenced by the kind of oil or the steel grade of the object to be measured and without using limited object with high-environment load.
Description
Technical field
The present invention relates to surface organic compound concentration measuring method that the concentration of the surface organic compound that is coated on lip-deep lubricated wet goods such as welding wire is measured.
Background technology
Usually in the manufacturing of welding wire etc., welding wire is being received into reel (spool) or packing tube (Pailpack) packing container of etc.ing before to its oiling.In this painting process, it is extremely important that oily adhesion amount is controlled in the specific scope, during low on fuel, can cause getting rusty, become difficult with certain speed feeding welding wire when making welding, opposite when oil mass is excessive, the burning gases of oil are blended in the weld metal, generation gas hole defect and make the strength degradation of weld part.Therefore, immediately oil mass is measured after the coating, when oil mass is not in specialized range, is needed rapidly the oil mass information feedback to be arrived the operating condition of apparatus for coating, thereby condition is revised.
Based on above-mentioned requirements, proposed a kind of oil mass in the past and carried out method for measuring (spy opens 2005-257553, the spy opens 2005-91306) welding wire surface.As this oil mass assay method, specifically there be (a) to use with the method for phenixin as the oil concentration analyzer that extracts solvent; (b) use the method for replacement fluorine Leon as the oil concentration analyzer that extracts solvent; (c) make tablet with ultrared materials such as absorption of K Br not, use the method for the direct catoptrical Infrared spectrophotometer (FTIR) of utilizing tablet surface.(d) with infrared ray direct irradiation determinand surface, detect direct catoptrical infrared measure; (e), infer the method that adhesion amount is arranged from the adhesion condition of the oil stain on filter paper surface with wiping welding wire surfaces such as filter paper.
Yet there is problem as follows in above-mentioned existing welding wire surface oil mass assay method.At first, the phenixin that (a) uses in the method is the restrictive substance of Montreal Protocol, only limits to basic purposes such as analysis, mensuration, to 2007 the year end this material use will be abrogated, can not use from now on.In addition, because be with oil with C-H combination device as determination object, the wavelength that can only measure the interatomic disance that is equivalent to the C-H combination is near the ultrared absorbance the 3.4 μ m, so can not be to PFPE (Perfluoropolyether), PTFE (polytetra-fluoroethylene; Teflon) etc. the adhesion amount that only has the lubricant of C-F combination is measured.
In (b) method, the solvent that is used to extract costs an arm and a leg, and all replacement fluorine Leons with C-Cl combination all are the depletion of the ozone layer materials, therefore becomes the possibility height of restriction object material from now on.This method is also identical with (a) method, can not measure the lubricating oil beyond the C-H oil.
In (c) method, after sherwood oil or acetone and other organic solvent stripping oil branch,, remove solvent and be configured as tablet afterwards with the KBr powder, measure oil mass by the ultrared absorbance that shines on the KBr tablet.The advantage of this method is that solvent is not limited to phenixin, on the contrary, evaporates, removes solvent and make the time that pre-treatment spent such as KBr tablet long, therefore makes rapidly and feeds back the difficulty that becomes to operating condition.
(d) method is employed to be the coating device etc. of steel plate, though this method is easy, because be the technology that is used for sheet material, is subjected to the restriction of the shape and the rugosity of determinand, so can not be used for columned welding wire.
(e) method is very easy, but quantitatively property is poor, is unsuitable for the oil mass management of the high high tension steel of hydrogen induced cracking susceptibility with welding wire etc.
In addition, in the so-called infrared spectroscopic analysis, the method of oriented above-mentioned (a) and (b), (c) is used the method through light like that, with use direct catoptrical method like that to the method for (d), in addition utilize the method for scattered reflection light in addition, but using the method for scattered reflection light is the method that can be used for the structure analysis of powder test portion, can not be used to have the mensuration of surface attachment substrate concentration of the determinand of curvature.
Summary of the invention
The present invention designs just in view of the above problems, its purpose is, the restriction of the kind of a kind of steel grade that is not subjected to determinand and oil is provided, do not use the restrictive substance of high carrying capacity of environment, can high precision and determine the surface organic compound concentration measuring method of the adhesion amount that is coated on the oil on the determinand easily.
Of the present invention organic compound substrate concentration as the welding wire surface of determinand is carried out method for measuring, be that cylinder or determinand cylindraceous seamlessly are arranged in the infrared radiation zone, be decided to be A at diameter with the infrared radiation zone, the external diameter of cylinder or described determinand cylindraceous is decided to be D, during width being set being decided to be B when many velamens are measured things and are arranged in the infrared radiation zone side by side, make it satisfy A/D 〉=2, the relation of B 〉=(A+D), the irradiation infrared ray is used to from the scattered reflection light of determinand the ultrared absorbance of specific wavelength be measured.
Said " surface organic compound concentration " is meant that welding wire per unit mass welding wire surface is attached with the organic compounds quality.
In this surperficial organic compound concentration measuring method, the organic compound that becomes determination object for example be the fatty acid amide of the aliphatic alcohol, meson acid acid amides of the fatty acid ester, oleic acid alcohol of the monovalent alcohol of the fatty glyceride of vegetable seed wet goods, rice bran wax etc. etc. etc., the mineral oils that do not have a polar bond do not have the bobbin oil of 2 heavy combinations or have 2 heavily combination polybutylene or do not have the PFPE of C-H combination.
Perhaps, the organic compound that becomes determination object for example is attached to the lip-deep PTFE of determinand (polytetrafluoroethylene teflon) by cementing agent.About the adhesion amount of these solid, by each accompanying material is made detection line, and can measure concentration accurately.
In addition, surface organic compound concentration measuring method of the present invention to described determinand irradiation infrared ray, is measured its absorbance from positive and negative both direction, measures the organic compound substrate concentration on described determinand surface according to its mean value.
Description of drawings
Fig. 1 is the mode chart that formation of the present invention is described.
Fig. 2 is the mode chart of the absorbance measurement method of expression embodiments of the present invention.
Fig. 3 is that expression is installed in the determinand on the support and the figure of standard test portion.
Fig. 4 is the figure of mensuration of the face side of expression support.
Fig. 5 is the figure of mensuration of the reverse side of expression support.
Fig. 6 is the curve map that expression is provided with the relation of width B and absorbance.
Fig. 7 is the figure that expression is measured from 4 directions.
Fig. 8 is the figure of an example of the oily absorption spectrum of expression.
Fig. 9 is the figure of an example of the inspection amount line of expression fatty glyceride coating welding wire.
Figure 10 is the mode chart of the existence of expression dope.
Figure 11 is the figure that only represents when a direction is measured oily adhesion amount.
Figure 12 is the figure of expression when positive and negative both direction is measured oily adhesion amount.
Embodiment
Below, embodiments of the present invention are described.As mentioned above, use the infrared spectroscopic analysis device of scattered reflection light to be used for the structure analysis of powder test portion all the time, normally measure in the mode that to serve as number μ m with particle diameter seamlessly be arranged in the ultrared irradiation area to the powder particle of 200 μ m.Therefore, be under the situation of welding wire at determinand as the present invention, use the infrared spectroscopic analysis device of scattered reflection light also inapplicable.
But, the present inventor person has carried out making great efforts repeatedly research to this, (diameter commonly used is in the experimental study that usability methods carried out of diffusion reflection pattern infrared spectroscopy device of cylindric or determinand cylindraceous such as 0.8～2.4mm) at the welding wire that the particle diameter of comparing the powder test portion is had very big diameter, find as shown in Figure 1, by being measured thing, many velamens are arranged as width greater than ultrared irradiation area, according to the suitably selected infrared radiation diameter of the diameter of determinand, can measure attachment concentration accurately.
Its reason may be thought of as when columned a plurality of determinands (welding wire) being placed side by side when arranging in the plane, shine the lip-deep light of test portion, between adjacent bonding wire, produce scattered reflection in the phase mutual interference, as have and reflected light is returned the plane of specific surface roughness.
The arrangement width (width is set) of determinand is narrower than under the situation of ultrared irradiating width, becomes error from the reflected light of not arranging the test portion part, can not obtain to measure fully precision.Therefore, width being set must be more than (irradiating width+determinand external diameter).
In addition, for the irradiation diameter, when the external diameter of determinand was big, the aligning method of measuring thing with respect to irradiation area was under rotational symmetry and the nonaxisymmetrical situation, and it is big that the error of infrared absorbance becomes.Therefore, need be according to the line footpath of determinand, suitably selected infrared radiation diameter.
The present invention just is being based on above-mentioned opinion and is designing, as shown in Figure 1, for the diameter A that makes the infrared radiation zone and the outer diameter D of determinand cylindric or cylindraceous (welding wire), and many velamens are measured things be arranged in being provided with between the width B in the infrared radiation zone, satisfy following relation
A/D≥2 (1)
B≥(A+D) (2)
Determinand cylindric or cylindraceous is arranged in the infrared radiation field, shines infrared ray, utilize the scattered reflection light of determinand, the ultrared absorbance of specific wavelength is measured.
Thus, can measure the organic compound substrate concentration on determinand surface.So, by the present invention, can not be subjected to the influence of kind of the steel grade and the oil of determinand, do not use the restrictive substance of high carrying capacity of environment, and the adhesion amount that is coated on the oil on the determinand is carried out high-precision measuring.
Fig. 2 is the mode chart of the optical system of the diffusion light reflection-type Infrared spectrophotometer used in the embodiments of the present invention of expression.The infrared ray that light source sends is injected concave mirror M3 by interferometer 1 pack through level crossing M1, M2, is shone the surface of test portion 2 after this concave mirror M3 pack.By the scattered reflection light of the surface reflection of test portion 2, after concave mirror M4 pack, be directed to detecting device 3 (with reference to figure 1) through level crossing M5, M6.
For example, with two test portions (determinand 2) and standard test portion 2a, be fixed on the support shown in Figure 34.That is, will not have the standard test portion 2a of attaching oil and determinand 2 to be installed on the support 4, for example, as shown in Figure 4,, absorbance will be measured with Infrared spectrophotometer with the order of standard test portion 2a → the 1st determinand 2 → the 2nd determinand 2.Secondly, support 4 is unloaded from determinator, as shown in Figure 5 that support 4 is inverted, with the order of standard test portion → determinand 1 → determinand 2, the face of reverse side is measured.At last, calculate the mean value (being 4 times mean value in this case) of measured value, thereby draw the surperficial oil mass of determinand 2.
Fig. 1 is near the figure after amplifying the test portion chamber among Fig. 2, and it is that the determinand 2 cylindric or cylindraceous of D is provided with width when being arranged in the infrared radiation zone that B represents many external diameters; A represents the diameter in ultraviolet radiation zone territory.
In the present invention, satisfy the condition of A/D 〉=2.When the value less than 2 of A/D, can be because the position difference of welding wire top in the infrared radiation zone, that is, and according to test portion being carried situation for axisymmetricly with respect to the infrared radiation zone, with the situation from axisymmetric position deviation, the value of absorbance produces great changes.Therefore, it is big that the deviation of measured value becomes, thereby can not carry out high-precision absorbance measurement.
In addition, in the present invention, satisfy the condition of B 〉=(A+D).As width (width is set) B that arranges determinand, when being narrower than ultrared irradiating width, the reflected light of not arranging the part of test portion forms error, thereby can not obtain to measure fully precision.Also have, only can transfer wide meeting to cause minute to prolong width is set.In addition, under the situation of (A+D)＞B 〉=A, along with the increase that width is set, absorbance can increase slightly, thereby causes measuring the error of precision.
Test portion is arranged as under (A+D) above situation (B 〉=(A+D)), even in the irradiation area outer edge, also the same with the irradiation area central portion, return reflected light as plane with particular surface rugosity, even being provided with the width absorbance, increase can not produce change yet.So need be made as B 〉=(A+D).
Become the organic compound of determination object of the present invention, fatty acid ester, aliphatic alcohol or the PFPE of fatty glyceride, monovalent alcohol for example arranged.These materials are effective feeding lubricants, need to use the inventive method to be controlled to be suitable adhesion amount.
In addition, these become the organic compound of determination object, also can adopt by cementing agent attached to the lip-deep PTFE (polytetra-fluoroethylene of determinand; Teflon).This PTFE also is the active principle as the feeding lubricant.
When measuring the organic compound substrate concentration of welding wire surface, be preferably from positive and negative both direction and shine infrared ray, measure its absorbance, measure the organic compound substrate concentration on described determinand surface by its mean value to welding wire.
Overlayed on the adhesion amount of the organic compound (oil) of welding wire surface, because of the coating process of oil changes on the circumferencial direction of welding wire.Figure 10 (a) is expression when by infusion process oil being coated with, the mode chart of the existence of oiling in the length direction right-angle cross-section of welding wire; The mode chart of the oily attachment state when Figure 10 (b) is the expression Electrostatic greasing.During by the infusion process oiling, the change of the adhesion amount of welding wire circumferencial direction is little, and when carrying out Electrostatic greasing, the change of the adhesion amount of welding wire circumferencial direction is big.
When by the FTIR method oil mass of welding wire surface being measured, the organism that adheres on can only the part (first half of welding wire circumferencial direction) to reflected infrared among Figure 11 is measured.Therefore, when only from a direction (only from the top) to electrostatic coating when the oily adhesion amount of welding wire surface is measured, under the influence of the adhesion amount change of the circumferencial direction of welding wire, the accurately situation of the oil mass of welding wire integral body can appear.
So, be preferably for the welding wire that is arranged in parallel, by behind a plurality of direction detections oil adhesion amounts, averaging, the influence that causes with the adhesion amount deviation that reduces the welding wire circumferencial direction.Thus, can assess the oily adhesion amount of welding wire integral body exactly.In this case, it is few more to think that deflection error is measured in increase more, but can cause the increase of minute and workload on the contrary.Present inventor person finds, as shown in figure 12, by many root beads silk is arranged on the support, measure from the front, simultaneously, change and positive and negatively measure once more from the negative, after 2 directions are measured oil mass, average, can obtain and direction is measured in per 90 ° of conversion, carry out the mensuration precision of mean time same degree after 4 direction detection oil masses.And as shown in figure 12, the counter-rotating pros and cons carries out the disposal route of twice oil mass mensuration, compares with the disposal route that per 90 ° of conversion mensuration direction is measured oil mass, and its workload is few.
(embodiment)
Secondly,, compare, effect of the present invention is described with the comparative example that exceeds zone of the present invention by making the embodiment that belongs in the scope of the invention.Fig. 6 is the expression welding wire that will scribble rapeseed oil (line footpath: 1.2mm) as determination object, use the diffusion light type infrared spectrophotometer of infrared radiation diameter 4.0mm, test portion is provided with the result curve figure that the relation of width and infrared absorbance is investigated.In the scope that width is (more than the 5.2mm) more than the A+D was set, absorbance demonstrated fixed value, when width being set being positioned at this zone, based on the inspection amount line of obtaining in advance, can obtain oil mass accurately.In the zone that the not enough A+D of width is set,, be difficult to obtain oil mass exactly along with the rising absorbance that width is set changes.
The method for making of this inspection amount line is as described below.At first, adopt infusion process to make the welding wire that scribbles fatty glyceride, with it as sample.By changing the oil concentration of dipping tank, the oily adhesion amount of welding wire is changed.And, welding wire focused in the vial measure its quality, behind organic solvent extraction oil,, make the KBr tablet behind the evaporative removal solvent with itself and KBr powder.Measure FTIR spectrum by penetrant method, thus the oil mass of measuring.
Then, welding wire is arranged in irradiation infrared ray in back on the test portion platform, measures infrared absorption spectrum, obtain-CH by reflected light
2The area of absorption peak.Carry out welding wire repeatedly and take, as shown in Figure 7, measure, obtain the mean value of peak area from 4 directions.Fig. 8 is an example of this oily absorption spectrum of expression.In addition, Fig. 9 represents that the fatty glyceride of obtaining as above-mentioned method is coated with an example of the inspection amount line of welding wire.Inspection amount line shown in Figure 9 represent oil mass and-CH
2The relation of the area of absorption peak, transverse axis are represented the oil mass (oil mass of the welding wire of every 10kg (g)) obtained by penetrant method, and the longitudinal axis is represented-CH
2The area of absorption peak.As shown in Figure 9, the relation that has linear function between peak area y and the oil mass x.
Following table 1 is that expression changes the size of irradiation area and welding wire and dope kind, the result that adhesion amount is investigated.In the situation of embodiments of the invention 1～19, the oil mass of obtaining by scattered reflection FTIR method (the inventive method) has good consistance with the measured value of the infrared measure that uses the KBr tablet, shows and has all carried out correct mensuration.
On the contrary, in comparative example 1～6, because width B narrow (B＜(A+D)) is set, the measured value by scattered reflection FTIR method oil mass of obtaining and the infrared measure that uses the KBr tablet produces deviation, is unsuitable.
In addition, in comparative example 7～9, because the radical few (A/D＜2) of determinand in the irradiation area, therefore can not carry out sufficient scattered reflection, compare by the measured value that scattered reflection FTIR method oil mass of obtaining and the FTIR method of using the KBr tablet are obtained, shown oil mass is few, shows to fail to carry out correct mensuration.
[table 1]
| Distinguish | The diameter A (mm) in infrared radiation zone | The outer diameter D of determinand (mm) | A/D ≥2 | A+D ≥B | B (mm) | The dope kind | Scattered reflection FTIR method oil mass (g/10kg) | Use the infrared measure oil mass (g/10kg) of KBr tablet | |
| Embodiment | 1 | 4 | 1.2 | 3.3 | 5.2 | 6 | Bobbin oil | 0.11 | 0.12 |
| 2 | 4 | 1.2 | 3.3 | 5.2 | 6 | Polybutylene | 0.33 | 0.31 | |
| 3 | 4 | 1.2 | 3.3 | 5.2 | 6 | Rapeseed oil | 0.51 | 0.55 | |
| 4 | 4 | 1.2 | 3.3 | 5.2 | 6 | Palm oil | 0.65 | 0.64 | |
| 5 | 4 | 1.2 | 3.3 | 5.2 | 6 | Rice bran is cured | 0.71 | 0.69 | |
| 6 | 4 | 1.2 | 3.3 | 5.2 | 6 | Oleyl alcohol | 0.82 | 0.82 | |
| 7 | 4 | 1.2 | 3.3 | 5.2 | 6 | Erucyl amide | 1.21 | 1.24 | |
| 8 | 4 | 1.2 | 3.3 | 5.2 | 6 | Stearic amide | 1.89 | 1.88 | |
| 9 | 4 | 1.2 | 3.3 | 5.2 | 6 | PFPE | 0.32 | 0.29 | |
| 10 | 4 | 1.2 | 3.3 | 5.2 | 6 | PTFE | 1.98 | 1.97 | |
| 11 | 4 | 0.8 | 5.0 | 4.8 | 5.6 | Rapeseed oil | 1.21 | 1.18 | |
| 12 | 4 | 1.4 | 2.9 | 5.4 | 7.0 | Rapeseed oil | 1.22 | 1.22 | |
| 13 | 4 | 1.6 | 2.5 | 5.6 | 8.0 | Rapeseed oil | 1.15 | 1.13 | |
| 14 | 7 | 0.8 | 8.8 | 7.8 | 8.0 | Rapeseed oil | 1.21 | 1.19 | |
| 15 | 7 | 0.9 | 7.8 | 7.9 | 9 | Rapeseed oil | 1.24 | 1.22 | |
| 16 | 7 | 1.2 | 5.8 | 8.2 | 8.4 | Rapeseed oil | 1.32 | 1.35 | |
| 17 | 7 | 1.6 | 4.4 | 8.6 | 9.6 | Rapeseed oil | 1.15 | 1.18 | |
| 18 | 3 | 0.8 | 3.8 | 3.8 | 4.0 | Rapeseed oil | 1.18 | 1.21 | |
| 19 | 3 | 1.4 | 2.1 | 4.4 | 5.6 | Rapeseed oil | 1.19 | 1.18 | |
| Comparative example | 1 | 4 | 0.9 | 4.4 | 4.9 | 4.5 | Rapeseed oil | 0.83 | 1.23 |
| 2 | 4 | 1.2 | 3.3 | 5.2 | 4.8 | Rapeseed oil | 0.78 | 1.291 | |
| 3 | 7 | 1.4 | 5.0 | 8.4 | 7.0 | Rapeseed oil | 0.86 | 1.25 | |
| 4 | 7 | 2.4 | 2.9 | 9.4 | 7.2 | Rapeseed oil | 0.92 | 1.23 | |
| 5 | 3 | 0.9 | 3.3 | 3.9 | 3.6 | Rapeseed oil | 0.95 | 1.23 | |
| 6 | 3 | 1.2 | 2.5 | 4.2 | 3.6 | Rapeseed oil | 1.03 | 1.17 | |
| 7 | 4 | 2.4 | 1.7 | 6.4 | 7.2 | Rapeseed oil | 0.89 | 1.26 | |
| 8 | 3 | 1.6 | 1.9 | 4.6 | 4.8 | Rapeseed oil | 0.67 | 1.23 | |
| 9 | 3 | 2.4 | 1.3 | 5.4 | 7.2 | Rapeseed oil | 0.78 | 1.22 |
Claims (4)
1. one kind is carried out method for measuring to the organic compound substrate concentration as the welding wire surface of determinand, it is characterized in that,
Determinand cylindric or cylindraceous seamlessly is arranged in the infrared radiation zone,
Be decided to be A at the diameter with the infrared radiation zone, external diameter cylindric or described determinand cylindraceous is decided to be D, during width being set being decided to be B when many velamens are measured things and are arranged in the infrared radiation zone side by side, satisfies the relation of A/D 〉=2, B 〉=(A+D),
The irradiation infrared ray is used to from the scattered reflection light of determinand the ultrared absorbance of specific wavelength be measured.
2. surface organic compound concentration measuring method according to claim 1 is characterized in that, the organic compound that becomes determination object is fatty acid ester, aliphatic alcohol or the PFPE of fatty glyceride, monovalent alcohol.
3. surface organic compound concentration measuring method according to claim 1 is characterized in that, the organic compound that becomes determination object is attached to the lip-deep teflon of determinand by cementing agent.
4. according to each described surface organic compound concentration measuring method in the claim 1～3, it is characterized in that, to described determinand irradiation infrared ray, measure its absorbance from positive and negative both direction, measure the organic compound substrate concentration on described determinand surface according to its mean value.
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| JPH02110347A (en) * | 1988-10-20 | 1990-04-23 | Teijin Ltd | Measuring method of adhering amount of oil to fiber |
| JP2002131305A (en) * | 2000-10-23 | 2002-05-09 | Sensu Kk | Method for simultaneously measuring concentration of a plurality of constituents by using detector tube and measuring instrument for the same |
| JP2002350342A (en) * | 2001-05-28 | 2002-12-04 | Advantest Corp | Method and apparatus for measuring surface state |
| JP2003181684A (en) * | 2001-12-19 | 2003-07-02 | Kobe Steel Ltd | Mig wire for welding aluminum or aluminum alloy material |
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| CN111971547B (en) * | 2018-03-30 | 2024-04-16 | 杰富意钢铁株式会社 | Powder ratio measuring device, powder ratio measuring system, and method for operating blast furnace |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN100580425C (en) | 2010-01-13 |
| JP4679486B2 (en) | 2011-04-27 |
| JP2008102044A (en) | 2008-05-01 |
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