CN107219185A - The assay method of sulfur content in a kind of electrode coating and flux-cored wire medicinal powder - Google Patents
The assay method of sulfur content in a kind of electrode coating and flux-cored wire medicinal powder Download PDFInfo
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- CN107219185A CN107219185A CN201710487729.XA CN201710487729A CN107219185A CN 107219185 A CN107219185 A CN 107219185A CN 201710487729 A CN201710487729 A CN 201710487729A CN 107219185 A CN107219185 A CN 107219185A
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- Prior art keywords
- flux
- cored wire
- sulfur content
- medicinal powder
- electrode coating
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 36
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 36
- 239000011593 sulfur Substances 0.000 title claims abstract description 36
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000003556 assay Methods 0.000 title claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 50
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 34
- 239000010937 tungsten Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 26
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 21
- 239000010959 steel Substances 0.000 claims abstract description 21
- 239000005864 Sulphur Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 9
- 238000011088 calibration curve Methods 0.000 claims description 5
- 238000011410 subtraction method Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 abstract description 26
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000003908 quality control method Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 239000011135 tin Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 abstract description 2
- 230000010076 replication Effects 0.000 abstract description 2
- 238000003466 welding Methods 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000004164 analytical calibration Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012764 semi-quantitative analysis Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 230000003019 stabilising effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Abstract
The present invention relates to a kind of assay method of sulfur content in electrode coating and flux-cored wire medicinal powder, using steel standard sample calibration instrument, the sulfur content of electrode coating or flux-cored wire medicinal powder is determined in high frequency infrared ray carbon sulphur analyser by adding tungsten, iron, tin metal fluxing agent;This method has that analytical procedure is simple, chemistry disruption is few, the characteristics of speed is fast, the degree of accuracy is high;The Determination Limit of the inventive method is 0.005% ~ 0.008%, the relative standard deviation of replication(RSD)No more than 8%, recovery of standard addition is between 80% ~ 104%, and method is accurate, quick, for the production of electrode coating and flux-cored wire medicinal powder, scientific research, using and quality control provide reliable guarantee.
Description
Technical field
The present invention relates to inorganic chemical analysis technical field of measurement and test, specifically a kind of electrode coating and flux-cored wire medicine
The assay method of sulfur content in powder.
Background technology
Welding is the high combination of important, high efficiency between metal, automaticity.As welding technique is in large-scale work
Extensive use in journey structural member association, the welding such as electrode coating and flux-cored wire medicinal powder is also sent out rapidly with pharmaceutical products
Exhibition.Electrode coating refers to coating of the extrusion on core wire surface, is made up of mineral matters such as oxide, fluoride etc.;Flux-cored wire medicine
Powder refers to be filled in the solder flux medicament in flux-cored wire, is made up of mineral matter, chemical products, ferroalloy, metal powder etc..Welded
Cheng Zhong, electrode coating is similar with the function of flux-cored wire medicinal powder, typically plays the effects such as slag making, stabilising arc, isolation air, is to determine
One of principal element of weldquality.
Element sulphur is the harmful element in weld seam, with sulphide inculsion in metal material, destruction metallization structure
Mechanical performance and decay resistance of continuity, easily reduction welding material etc..Therefore, control and accurate analysis electrode coating and medicine
Sulfur content in core welding wire medicinal powder, welding quality control and engineer applied have important directive significance.
Applicant by retrieval find, both at home and abroad there is not yet in electrode coating and flux-cored wire medicinal powder analysis of sulfur content phase
Close research report, and its product type is numerous, composition and nature difference are larger, do not have yet can be for reference electrode coating and medicine
Core welding wire medicinal powder standard sample, this to the production of the product, scientific research, using and quality control bring many difficulties.Existing
In technology, we can be determined using pressed powder-x ray fluorescence spectrometry and X-ray photoelectron spectroscopy electrode coating and
Sulfur content in flux-cored wire medicinal powder, but above two method belongs to semi-quantitative analysis, the error for determining sulphur is very big, it is difficult to full
The accurate quantitative analysis demand of sufficient sulfur content especially low sulfur content.
To solve the above problems as early as possible, sulphur in a kind of fast and accurately measure electrode coating and flux-cored wire medicinal powder is set up
The method of content has important practical significance.
The content of the invention
Belong to semidefinite for the above-mentioned method for determining the sulfur content in electrode coating and flux-cored wire medicinal powder in the prior art
Amount analysis, the error for determining sulphur is very big, it is difficult to the problems such as meeting the accurate quantitative analysis demand of sulfur content especially low sulfur content,
The present invention provides a kind of assay method of sulfur content in electrode coating and flux-cored wire medicinal powder.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
The assay method of sulfur content, comprises the following steps in a kind of electrode coating and flux-cored wire medicinal powder:
Step one:Using steel standard sample calibration instrument, the system blank value of tin+tungsten is determined and deducted first;0.1 is weighed again
~ 0.5 g steel standard samples, add tin+tungsten and make fluxing agent, determine the sulfur content of steel standard sample, illustrate by instrumentation
Calibration instrument or the calibration curve for setting up element sulphur;
Step 2:The method blank value of iron+tin+tungsten is determined, signal intensity subtraction method blank value is pressed according to instrumentation explanation;
Step 3:0.05 ~ 0.30g electrode coatings to be measured or flux-cored wire medicinal powder sample are weighed in the crucible for being pre-placed pure iron
In, tin+tungsten fluxing agent is added, the sulfur content of actual sample is determined.
The addition of the fluxing agent is respectively:Iron:0~0.5 g;Tin:0~0.5 g;Tungsten:1.5~2.5 g.
The amount of weighing of the steel standard sample is:0.3~0.5 g.
Electrode coating and flux-cored wire the medicinal powder sample particle diameter is:80 mesh or 100 eye mesh screens are crossed, the amount of weighing is:0.10~
0.15 g。
The addition sequence of the sample and fluxing agent is:Iron+sample+tin+tungsten.
Beneficial effects of the present invention:
The assay method of sulfur content in electrode coating and flux-cored wire medicinal powder that the present invention is provided, is calibrated using steel standard sample
Instrument, electrode coating or flux-cored wire medicine are determined by adding tungsten, iron, tin metal fluxing agent in high frequency infrared ray carbon sulphur analyser
The sulfur content of powder;This method has that analytical procedure is simple, chemistry disruption is few, the characteristics of speed is fast, the degree of accuracy is high;The inventive method
Determination Limit be 0.005% ~ 0.008%, the relative standard deviation of replication(RSD)No more than 8%, recovery of standard addition between
80% ~ 104%, method is accurate, quick, for the production of electrode coating and flux-cored wire medicinal powder, scientific research, using and quality control provide
Reliable guarantee.
Embodiment
With reference to embodiment, the present invention is further elaborated.
The assay method of sulfur content, comprises the following steps in a kind of electrode coating and flux-cored wire medicinal powder:
Step one:Using steel standard sample calibration instrument, the system blank value of tin+tungsten is determined and deducted first;0.1 is weighed again
~ 0.5 g steel standard samples, add tin+tungsten and make fluxing agent, determine the sulfur content of steel standard sample, illustrate by instrumentation
Calibration instrument or the calibration curve for setting up element sulphur;
Step 2:The method blank value of iron+tin+tungsten is determined, signal intensity subtraction method blank value is pressed according to instrumentation explanation;
Step 3:0.05 ~ 0.30g electrode coatings to be measured or flux-cored wire medicinal powder sample are weighed in the crucible for being pre-placed pure iron
In, tin+tungsten fluxing agent is added, the sulfur content of actual sample is determined.
Its principle is:A certain amount of sample and metal fusing agent(Such as tungsten, iron, tin)With high frequency electromagnetic field coupling, whirlpool is produced
Flow and generate heat, sample is fully burnt, the sulfide, free sulphur and organic sulfur in sample are oxidized to SO2Gas, sulfate quilt
It is pyrolyzed as SO3And it is further broken into SO2, carried by oxygen and enter detection SO in infrared pond after removing dust purification2Characteristic absorption peak
Intensity, so as to obtain the sulfur content in sample.Wherein, sample size, the consumption of fluxing agent and addition sequence, standard sample etc. are
High-frequency welded H steel is influenceed to determine the essential condition of carbon, sulphur accuracy and traceability.
Specific embodiment
Instrument:Carbon and sulfur analytical instrument(German ELTRA CS-800), condition of work:The MPa of oxygen pressure about 0.25, oxygen stream
About 180 L/h are measured, the maximum analysis time is 50 s, and minimum analysis time is 30 s.
Material and reagent
Ceramic crucible and crucible cover, using preposition in box-type high-temperature furnace, be warming up to 1000 DEG C of h of calcination 4 ~ 6, cool to the furnace
Room temperature, take out in drier preserve, it is standby.
Common oxygen:V/V≥99.2%;High purity oxygen gas:V/V≥99.999%.Tungsten particle:Purity >=99.95%,w(S)≤
0.0002%;Pure iron(Consider shape to be worth doing):Purity >=99.95%,w(S)≤0.0005%;Tin grain:Purity >=99.99%,w(S)≤
0.0005%。
Steel standard sample:Stainless steel 316 L YSB S 20313a-2013:w(S)=0.0020%;YSB C 11140a-
2011:w(S)=0.0025%;YSB C 20125-2005:w(S)=0.0051%;Pure iron GBW 01404a:w(S)=0.0063%;
15Mn YSB C 11128-99:w(S)=0.010%;20MnSi GBW(E) 010029:w(S)=0.013%;25# steel YSB C
11110-93:w(S)=0.018%;YSB C 11116:w(S)=0.020%;10# steel YSB C 1110a-93:w(S)=0.024%;
YSB C 11123-95:w(S)=0.039%;Automatic steel YSB C 11111b-99:w(S)=0.121%.Above-mentioned series standard sample
Product are used for instrument calibration or set up the calibration curve of sulphur.
The assay method of sulfur content, comprises the following steps in a kind of electrode coating and flux-cored wire medicinal powder:
Step one:Instrument calibration:Electrode coating, flux-cored wire medicinal powder are still without standard sample.The present invention uses steel standard sample
Product calibration instrument.Specific method is as follows:Determine first and deduct 0.20 g tin+1.7 g tungsten of grain by signal intensity integrated peak areas
The system blank value of grain.The serial steel standard samples of 0.3 ~ 0.5 g are weighed again, are added 0.20 g tin+1.7 g tungsten particles of grain, are set up
The calibration curve of element sulphur.System blank and standard sample parallel determination 2 ~ 3 times.The absolute mass of sulphur is horizontal stroke using in standard sample
Coordinate, the signal intensity integrated peak areas of the release profiles of sulphur carries out linear regression for ordinate, and linearly dependent coefficient isR 2=
0.999, linear relationship is good;
Step 2:The deduction of method blank value:The method for determining 0.30g ~ 0.50g pure iron+0.20g tin grain+1.7g tungsten particles first
Blank value;Method blank parallel determination 2 ~ 3 times, signal intensity integrated peak areas subtraction method blank is pressed according to instrumentation explanation
Value;
Step 3:The measure of actual sample:The g testing samples of 30 g ~ 60 are taken to crush the s of 2 s ~ 5 through disc type vibro-grinding instrument(Or make
It is fully ground with agate mortar), the sample after crushing or grinding should cross 80 mesh or 100 mesh shine net, be subsequently placed in 105 ~ 110 DEG C
Dry after 1 h with drier cooling, it is standby.Sample is weighed after 0.10 ~ 0.15 g processing in being pre-placed 0.30 ~ 0.50 g
In the crucible of pure iron, 0.2 g tin+1.7 g tungsten particles of grain are added, the sulfur content of actual sample is determined.
The detection limit and Determination Limit of the inventive method
Sample quality is in terms of 150 mg, and empirically method determines the method blank of g tin+1.7 g tungsten particles of grain of 0.3 g pure iron+0.2
Value, parallel determination 10 times.By 3 times of blank value standard deviation and 10 times of difference computational methods detection limits and Determination Limit.As a result
It is listed in table 1.
The Determination Limit of the inventive method is 0.005% ~ 0.008%.Method blank value and detection limit of the oxygen purity to sulphur
Existing with Determination Limit influences, and is preferably high purity oxygen gas when analyzing low sulfur content.
The detection limit of table 1 and Determination Limit
The precision test of the inventive method
The sulfur content of electrode coating or flux-cored wire medicinal powder sample is determined by determination step, 2 are the results are shown in Table.By table 2, the measure of sulphur
As a result relative standard deviation(RSD)No more than 8%, the precision of method is preferable.
The analysis result of sulphur in the actual sample of table 2
The recovery of standard addition experiment of the inventive method
The system blank value of 0.20 g tin+1.7 g tungsten particles of grain is determined and deducted first.Accurately weigh 0.10 g electrode coatings and medicine
Core welding wire medicinal powder actual sample, and input sample quality, add 0.3 ~ 0.5 g steel standard samples(YSBC11140a-
2011, YSBC20125-2005, GBW01404a, YSBC11128-99, GBW (E) 010029)Mark-on mixing is constituted instead of pure iron
Thing, adds 0.2 g tin+1.7 g tungsten particles of grain, the sulfur content of mark-on mixture is determined by determination step, and according to the data meter of table 2
The sulphur background amount in actual sample is calculated, sulphur mark-on amount is calculated according to the standard sample added.Recovery test result is listed in table
3.By table 3, the rate of recovery is between 80% ~ 104%, in compared with zone of reasonableness.
The recovery test result of the sulphur of the sample of table 3
Influence of the fluxing agent species to the measure of sulphur in sample
Implementation of the species of fluxing agent to the present invention has important influence.To be better understood from applying the present invention, to fluxing
The implementation of agent is done to be explained in detail as follows.
Suitable tungsten, iron, stannum fluxing agent species and addition sequence is selected to be to ensure that sample can be melted completely, sulphur is released
Entirely with the key of Accurate Determining.Wherein, tungsten play heating, ignite, it is fluxing, beneficial to SO2The effect of release, iron can play magnetic conduction work
With tin can reduce the fusing point of combustion system.
Experiment is found, in the case of tungsten fluxing agent, iron, tin, the amount of being optionally added of sample and the equal nothing of order of addition
Method is ignited sample, and the measured value of sulphur is extremely relatively low.After 1.5 g tungsten of addition make fluxing agent, the molten bath after sample measure is more
Smooth, smooth, without obvious pit or vigorous splash phenomenon, the release profiles of sulphur are in normal distribution, tungsten, iron, the consumption of tin substantially
And influence of the addition sequence to the measured value and stability of sulphur is not very obvious.But polynary fluxing action is slightly better than single fluxing agent,
It is thus determined that fluxing agent consumption is iron:0 ~ 0.5 g, tin:0 ~ 0.5 g, tungsten:1.5~2.5 g.It is preferred that, fluxing agent consumption and add
It is the g tungsten of+0.2 ~ 0.4 g tin of+0.10 ~ 0.15 g samples of 0.3 ~ 0.5 g iron+1.5 ~ 2.0 to enter order.
Claims (5)
1. the assay method of sulfur content in a kind of electrode coating and flux-cored wire medicinal powder, it is characterised in that comprise the following steps:
Step one:Using steel standard sample calibration instrument, the system blank value of tin+tungsten is determined and deducted first;0.1 is weighed again
~ 0.5 g steel standard samples, add tin+tungsten and make fluxing agent, determine the sulfur content of steel standard sample, illustrate by instrumentation
Calibration instrument or the calibration curve for setting up element sulphur;
Step 2:The method blank value of iron+tin+tungsten is determined, signal intensity subtraction method blank value is pressed according to instrumentation explanation;
Step 3:0.05 ~ 0.30g electrode coatings to be measured or flux-cored wire medicinal powder sample are weighed in the crucible for being pre-placed pure iron
In, tin+tungsten fluxing agent is added, the sulfur content of actual sample is determined.
2. the assay method of sulfur content in electrode coating as claimed in claim 1 and flux-cored wire medicinal powder, it is characterised in that:
The addition of the fluxing agent is respectively:Iron:0~0.5 g;Tin:0~0.5 g;Tungsten:1.5~2.5 g.
3. the assay method of sulfur content in electrode coating as claimed in claim 1 and flux-cored wire medicinal powder, it is characterised in that:
The amount of weighing of the steel standard sample is:0.3~0.5 g.
4. the assay method of sulfur content in electrode coating as claimed in claim 1 and flux-cored wire medicinal powder, it is characterised in that:
Electrode coating and flux-cored wire the medicinal powder sample particle diameter is:80 mesh or 100 eye mesh screens are crossed, the amount of weighing is:0.10~0.15 g.
5. the assay method of sulfur content in electrode coating as claimed in claim 1 and flux-cored wire medicinal powder, it is characterised in that:Institute
The addition sequence for stating sample and fluxing agent is:Iron+sample+tin+tungsten.
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