CN106979945A - A kind of method of Zn content in measure zincizing agent - Google Patents
A kind of method of Zn content in measure zincizing agent Download PDFInfo
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- CN106979945A CN106979945A CN201710271342.0A CN201710271342A CN106979945A CN 106979945 A CN106979945 A CN 106979945A CN 201710271342 A CN201710271342 A CN 201710271342A CN 106979945 A CN106979945 A CN 106979945A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000011701 zinc Substances 0.000 claims abstract description 120
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 59
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 26
- 238000005259 measurement Methods 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- 238000002203 pretreatment Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 238000002386 leaching Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 238000011088 calibration curve Methods 0.000 claims abstract description 10
- 238000000682 scanning probe acoustic microscopy Methods 0.000 claims abstract description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 58
- 235000016804 zinc Nutrition 0.000 claims description 57
- 239000000523 sample Substances 0.000 claims description 45
- 239000011521 glass Substances 0.000 claims description 28
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 28
- 239000012085 test solution Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000006184 cosolvent Substances 0.000 claims description 17
- 239000012488 sample solution Substances 0.000 claims description 17
- 230000003595 spectral effect Effects 0.000 claims description 17
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical class [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 12
- 239000012498 ultrapure water Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 8
- 238000010129 solution processing Methods 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 238000000889 atomisation Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 5
- 239000010425 asbestos Substances 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 230000005499 meniscus Effects 0.000 claims description 5
- 238000005457 optimization Methods 0.000 claims description 5
- 229910052895 riebeckite Inorganic materials 0.000 claims description 5
- 239000003381 stabilizer Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 238000011156 evaluation Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000000112 cooling gas Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000006210 lotion Substances 0.000 claims description 2
- QCAWEPFNJXQPAN-UHFFFAOYSA-N methoxyfenozide Chemical compound COC1=CC=CC(C(=O)NN(C(=O)C=2C=C(C)C=C(C)C=2)C(C)(C)C)=C1C QCAWEPFNJXQPAN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- -1 melt leaches Substances 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000010790 dilution Methods 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- 238000004445 quantitative analysis Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 14
- 229910000831 Steel Inorganic materials 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 12
- 239000010959 steel Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 238000009614 chemical analysis method Methods 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 238000005246 galvanizing Methods 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 5
- 238000004448 titration Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 238000004993 emission spectroscopy Methods 0.000 description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011133 lead Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229920001895 acrylonitrile-acrylic-styrene Polymers 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000005375 photometry Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010421 standard material Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000004210 cathodic protection Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 238000005479 sherardizing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 230000007306 turnover Effects 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Plasma & Fusion (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of method that Zn content in zincizing agent is determined with inductively coupled plasma atomic emission spectrometer, belong to technical field of chemical detection, it includes, and sample is weighed, pre-treatment melting, melt leaching, sample processing, dilution constant volume, wavelength selection, Zinc standard solution is prepared, prepared by calibration curve, ICP Atomic Emission Spectrometer AESs are detected, the calculating of analysis result and precision.Realize that zincizing agent sample pre-treatment dissolving is quick, Zinc standard solution prepares that matching is strong, anti-Matrix effects ability is strong, detection process is easily mastered, testing result is accurately and reliably.Measurement range：W (Zn) 20.00%~60.00%.The present invention is to the product quality of raising zincizing agent, production efficiency, there is provided solid foundation for reduction production cost；For the quick and precisely quantitative analysis of zinc in zincizing agent, there is provided reliable basis.Detection field top standard is reached.
Description
Technical field
It is a kind of with inductively coupled plasma atomic emission spectrometer measure zincizing agent the present invention relates to field of chemical detection
The ICP Atomic Emission Spectrometer AES quantitative analysis methods of Zn content in the method for middle Zn content, more particularly to a kind of zincizing agent, are determined
Scope：W (Zn) 20.00%~60.00%.
Background technology
The medium referred to as zincizing agent being made up of the zinc powder or addition energizer that can produce active zinc atom with filler.It is main
It is aluminum oxide, zinc agent, nickel powder, ammonium fluoride etc. to want constituent.
The principle of powder zincizing technology is that zincizing agent and steel piece are placed in Sherardizing furnace, 400 DEG C or so are heated to,
Active zinc atom then permeates to steel piece from outward appearance to inner essence.At the same time, iron atom spreads from inside to outside, and this is just in steel system
The top layer of part forms zinc-iron intermetallic compound, i.e. zinc coat.Zinc coat has electrode potential more more negative than ferrous materials, to work
Part forms a kind of good cathodic protection layer.Therefore, zincizing be improve metal material corrosion resistance it is most economical, most adopt extensively
Means of defence.Compared with electrogalvanizing, zinc coat has higher case hardness and wearability.
Powder zincizing product it is functional, summed up following characteristics：
One is that corrosion resistance is strong.Burn into corrosion is the natural enemy of ferrous materials.It is estimated that world's output of steel there are about ten/
One is lost in burn into corrosion.Corrode the economic loss caused to China annual at least more than 40,000,000,000 yuan.It was verified that in sea
Under a variety of environment such as foreign air, severe industrial atmosphere, the corrosion resistance of zinc coat is better than heat, electrogalvanizing and stainless steel.Same
Plant in industrial atmosphere, Corrosion of Stainless Steel 600 days, surface is just covered with rust spot, and galvanizing production corrodes more than 1600 days, and its surface does not have one
Point rusty stain.
Two be that wear-resisting, antifraying property is good.Zinc coat case hardness can reach HV250~400, and heat, electrogalvanizing product
Surface is pure zinc, and coating hardness is only HV70 or so, therefore zincizing specific heat, electrogalvanizing are wear-resisting and antifraying property is much better.
Three be to produce substantially pollution-free.In general, zincizing production pre-treatment only with shot-blasting machine derust edible vegetable oil,
And use bag-type dust.Using oil fuel as main energy sources in production, using circulating combustion smokeless emission technology.Powder zincizing technology
Ooze, produced without zinc fume for zinc solid, workpiece is permeated and separated in closed utensil again with auxiliary agent, to surrounding environment
Do not pollute.
Four be zinc consumption than relatively low.It is reported that, the zinc consumption ton product of galvanizing is 100kg or so, and powder oozes
Zinc is only 30kg or so, only accounts for the 30% of galvanizing.In addition, also corroding the hard nut to crack of this galvanizing without zinc pot.
Five be that can realize composite protective after painting.The zinc coat of zincizing product is uniform, and is one-level with the adhesion of paint.
The corrosion resistance of its composite armor is superior to heat, electrogalvanizing and zinc coat.
Six be that the steel product handled through zincizing does not influence the mechanical performance of material.The temperature of zincizing processing is lower than galvanizing
(100~280) DEG C.At a temperature of this, the hydrogen atom of suction steel matrix has spread effusion.Therefore, the danger without hydrogen embrittlement in the application
Evil, is also avoided that some high intensity parts such as spring the drawbacks of mechanical performance declines caused by treatment temperature height.
The application prospect of zincizing product：The performance advantage of zincizing product, determines that it applies wide, remarkable benefit.Such as outdoor
The parts such as steel construction and fastener, freeway guardrail, bridge, hot-water heating utensil, architectural hardware, automobile, engineering machinery.Powder
Anti-corrosion, high temperature resistant parts in the engineering such as metallurgical product and chemical industry, ocean, metallurgy, generating can all be produced using zincizing steel
Product, its economic benefit is very considerable.Service life such as galvanizing guardrail is generally 6 years.And zincizing guardrail alloying layer thickness (90
~100) μm, it can protect 30 years and not corrode, without big maintenance.It is estimated that with every kilometer of freeway guardrail, (row of two-way lane 4 protects
Column) to be counted using 30 years, its total galvanizing is more than 680,000 yuan, and zincizing is only with more than 230,000 yuan, and the former is nearly 3 times of the latter.According to relevant portion
Door is counted a few years ago, and national 70,000 kilometers of railways are used for railway nail and pour oily maintenance cost up to more than 400,000,000 yuan every year.According to zincizing road
Nail, exempts from overhaul in 30 years, can save more than 120 hundred million yuan for country.It is therefore seen that, powder zincizing technology can create huge warp for country
Benefit of helping and social benefit, such as plus raising resource utilization, the income of environmental protection each side, the tribute of powder zincizing technology
Offer very notable.
Powder zincizing technology comes from Britain and the former Soviet Union.Since nineteen nineties, the expert of relevant department of China
By concentrating on studies and testing, powder zincizing technology, serial complete set of equipments and powder zincizing product are successfully developed, is obtained
The utility model such as powder zinc impregnation equipment, furnace body rotary powder zinc penetration equipment and powder zincizing screw-thread steel, tubing and section bar country
Patent, technology guarantee is provided to popularize this new technology in an all-round way in China.
In order to meet the production requirement of zincizing agent novel product, it is necessary in strict control zincizing agent the content of Zn-ef ficiency and
Addition, this has undoubtedly gone out a difficult problem to chemical analysis worker, and the exploitation for its detection technique proposes challenge.
Inquired about by Chongqing City's standard information service network, China closes in steel and its alloy, aluminium and aluminium alloy, copper and copper
Detection technique comparative maturity in terms of golden, zinc and kirsite, magnesium and magnesium alloy etc., the standard detection side for the issue that goes through at present
Method has about 1200 kinds.
With detecting that the relevant criterion of Zn content has：
(1) steels of GB 223.51-87 and the bromo- PADAP photometries of alloy analysis method 5- determine zinc amount, determine model
Enclose：W (Zn) 0.0015%~0.005%；
(2) part of measure the 12nd of the steels of GB/T 20127.12-2006 and alloy trace element：Flame Atomic Absorption Spectrometry light
Spectrometry determines Zn content, measurement range：W (Zn) 0.0005%~0.05%；
(3) lead of GB/T 4103.11-2012 and the part of metal chemical analysis method the 11st：The measure flame of zinc amount is former
Sub- absorption spectrometry, measurement range：W (Zn) 0.0003%~0.061%；
(4) copper of GB/T 5121.11-2008 and the part of copper alloy chemical analysis method the 11st：The assay method of Zn content
One flame atomic absorption spectrometry, measurement range：W (Zn) 0.0001%~2.01%；The 4- methyl of the method two-extraction point of pentanone -2
From-Na2EDTA titrations, measurement range：W (Zn) 2.00%~6.00%；
(5) copper of GB/T 5121.28-2010 and the part of copper alloy chemical analysis method the 28th：Chromium, iron, manganese, cobalt, nickel,
Zinc, arsenic, selenium, silver, cadmium, tin, zinc, tellurium, zinc, Determine trace Bismuth inductively coupled plasma mass spectrometry, measurement range：w(Zn)
0.0001%~0.0050%；
(6) lead of GB/T 4103.16-2009 and the part of metal chemical analysis method the 16th：Copper, silver, bismuth, arsenic, antimony,
The measure photo-electronic directly reading emission spectrometry of tin, zinc amount, measurement range：W (Zn) 0.00025%~0.0046%；
(7) (1~12) -2010 zinc of GB/T 12689. and kirsite chemical analysis method；
(8) magnesium of GB/T 13748.15-2013 and the part of magnesium alloy chemical analysis method the 15th：The measure of Zn content
The flame atomic absorption spectrometry of method one, measurement range：W (Zn) 0.10%~10.00%；
The PAN AASs of method two, measurement range：W (Zn) 0.0050%~0.100%；
The titration of method three, measurement range：W (Zn) 0.10%~8.0%；
(9) aluminium of GB/T 20975.8-2008 and the part of aluminum alloy chemically analysis method the 8th：The assay method one of Zn content
EDTA titrations, measurement range：W (Zn) 0.10%~14.0%；The flame atomic absorption spectrometry of method two, measurement range：w
(Zn) 0.001%~6.00%；
(10) zinc of GB/T 26042-2010 and kirsite chemical analysis method photoelectric emission spectrometry
(11) part of the tin of GB/T 3260.8-2013 chemical analysis method the 8th：The measure flame atomic absorption spectrometry of zinc amount
Method, measurement range：W (Zn) 0.00021%~0.0049%；
(12) cast bearings of YS/T 475.7-2005 alloy analysis method lead, copper, iron, bismuth, zinc, the measure of cadmium amount
Atomic absorption spectrography (AAS), measurement range：W (Zn) 0.0005%~0.20%；
(13) aluminum oxide of GB/T 6609.4-2004 chemical analysis method and method for measuring physical properties phenanthrolene light
Degree method determines ferric oxide content, measurement range：w(Fe2O3) 0.0005%~0.20%；
(14) zinc powders of GB/T 6890-2012
The measure Na of the full zinc amount of appendix A2EDTA titrations, measurement range：W (full Zn) 90.00%~99.08%；
The measure permanganimetric method of Appendix B metallic zinc amount, measurement range：W (metal Zn) 88.75%~99.25%.
However, above standard method of analysis, has used the bromo- PADAP photometries of 5-, PAN AASs, NITRATE BY FLAME ATOMIC to inhale
Receive spectroscopic methodology, the 4- methyl-extract and separate of pentanone-2-Na2EDTA titrations, inductively coupled plasma mass spectrometry, photo-electronic directly reading
Emission spectrometry, inductively coupled plasma-emission spectrometry, permanganimetric method etc., major defect has：Detection process is answered
Miscellaneous, detection elements are seriously polluted, and detection time is up to more than 16h；Or, it is necessary to use large-scale precision ICP-MS instruments；Or,
Need to prepare a variety of single element standard liquids consistent with zincizing agent matrix, and prepare and divide access kind elemental standard solution to build
The time of day-mark directrix curve is very long and manipulation strength is especially big, particularly experienced many effort, although standard curve is linearly very
It is good, but because Matrix Match is poor, the testing result obtained by standard curve is often unsatisfactory；For zincizing agent
For, when the molten sample technology of the pre-treatment using above-mentioned standard method, sample dissolving is incomplete, it is impossible to obtain accurate zinc content
Test result.For determining Zn content in zincizing agent, the zincizing agent standard substance close with selecting is purchased, it is bent to set up work
Line, this can not accomplish.That is, without suitable zincizing agent series standard material, it is impossible to meet Zn-ef ficiency in zincizing agent
The accurate detection requirement of content.
The ICP Atomic Emission Spectrometer AES assay method (measurement ranges of Zn-ef ficiency content in zincizing agent are not found now：w(Zn)
20.00%~60.00%).In addition, in company standard method, the applicable detection method of correlation is not found yet.For at present,
As the exploitation of the ICP Atomic Emission Spectrometer AES detection methods of zincizing agent Zn content, still belong to blank.
The content of the invention
There is provided one kind inductively coupled plasma for the problem of purpose of the present invention is exactly to solve above-mentioned background technology
The method that Atomic Emission Spectrometer AES determines Zn content in zincizing agent.
In the method for the present invention, sample is contained in platinum crucible, is added potassium pyrosulfate, is mixed with thin wire.In high temperature
In resistance furnace, 700 DEG C~750 DEG C melting samples are heated to, melt complete to sample.Add hydrochloric acid solution leaching melt.Will examination
Material solution is heated to boiling, and cosolvent is added dropwise.Cool down test solution.Certain volume is diluted to the water of two grades and above rank, is mixed.
With Zn-ef ficiency standard liquid and potassium pyrosulfate preparation solution, calibration curve is prepared, on ICP Atomic Emission Spectrometer AESs, in being recommended
Wavelength at, measurement blank test and test solution in Zn-ef ficiency emitted luminescence intensity, shown automatically in sample by detecting instrument equipment
The mass concentration of zinc, then obtains the mass fraction of zinc in sample by conversion again.
Zinc contains in a kind of measure zincizing agent using inductively coupled plasma atomic emission spectrometer involved in the present invention
The method of amount, including sample is weighed, pre-treatment melting, melt leaching, test solution processing, dilution constant volume, wavelength selection, zinc standard it is molten
Liquid is prepared, calibration curve prepares (using potassium pyrosulfate preparation solution), the detection of ICP Atomic Emission Spectrometer AESs, the calculating of analysis result
And precision.
Comprise the following steps that：
Step one：Sample is weighed
A ten thousandth electronic balance is used, 0.1000g zincizing agent samples is weighed, is placed in 50mL platinum crucibles；
Step 2：Pre-treatment melts
In the platinum crucible for being loaded with zincizing agent sample, about 2g potassium pyrosulfates are added, are mixed with thin wire.In high-temperature electric
Hinder in stove, be heated to 700 DEG C~750 DEG C melting samples, melt complete to sample；Take out, be placed on heat-resisting asbestos board, be cooled to
Room temperature；
Step 3：Melt leaches
Melt leaching includes the producing of water, the preparation of hydrochloric acid solution, the preparation of cosolvent solution and sample and dissolved.
Step 4：Test solution processing
Test solution processing is including boiling, cosolvent is prepared, cosolvent is added dropwise, test solution is cooled down；
Step 5：Dilute constant volume
The sample solution of room temperature will be cooled to after sample dissolution process, be transferred in 100mL volumetric flasks, in transfer process
In, inserted with a glass bar in volumetric flask, tilt the beaker for containing sample solution, beaker is tight-lipped to lean on glass bar, makes solution edge
Glass bar is slowly flowed into, and glass bar lower end will be close to bottleneck inwall, but should not be too near to bottleneck, in order to avoid have solution spilling.
Step 6：Wavelength is selected
Inductively coupled plasma atomic emission spectrometer (ICP-AES) is opened, more than 2h is preheated；According to instrument specification
Instrument condition of work is optimized, after the optimization of instrument condition of work, in element determination wavelength spectral line, according to Zn-ef ficiency content
Scope, linear relationship, the rate of recovery, testing result accuracy are considered, and selection is suitable to determine wavelength.Selected measure
Wavelength is：Zn 202.548nm、213.856nm.
Step 7：Zinc standard solution is prepared
1.0000g metallic zincs (>=99.9%) are dissolved by heating in 50mL salpeter solutions (1+1), moved into after cooling
In 100mL volumetric flasks, then add 50mL salpeter solutions (1+1), with two grades and the water of above rank, when being diluted to about 3/4 volume,
Volumetric flask yawing (is sure not to reverse and shaken) several times, makees preliminary mix.Then proceed to add the water of two grades and above rank, nearly mark
During line, carefully it is added dropwise with dropper, untill the minimum point and graticule of the lower meniscus of Zn-ef ficiency solution are tangent；Cover tightly
Glass stopper；Left index finger pins glass stopper, and right hand finger tip withstands bottom of bottle edge, and volumetric flask the other way around and is shaken, then
The other way around, the bubble in solution is risen to top, so repeatedly 10 times~15 times, mix, this is Zn-ef ficiency standard liquid
(1mL zinc containing 10mg).
Step 8：It is prepared by calibration curve
In 6 50mL platinum crucibles, about 2g potassium pyrosulfates are separately added into, are mixed with thin wire；Same sample is operated below
Pre-treatment melting, melt leaching, sample dissolving；Be separately added into 0,2,3,4,5,6mL Zn-ef ficiency standard liquids, it is dilute with ultra-pure water
Release to scale, mix.
Step 9：ICP Atomic Emission Spectrometer AESs are detected
Click on plasmatorch to automatically begin to igniting, instrument operational factor is confirmed after igniting in normal range (NR), atomization system
System and plasma torch are working properly, more than stabilizer instrument 15min.
Step 10：The calculating of analysis result
According to the mass concentration of zinc in sample solution, represented with mg/mL, to calculate the mass fraction of zinc in zincizing agent；
Step 11：Artificial synthesized standard specimen checking
Step 12：Production examination analysis result
Using a kind of ICP detection methods of Zn-ef ficiency content in zincizing agent, detection and precision have been carried out to material to be tested
Experiment.
A kind of method that Zn content in zincizing agent is determined with inductively coupled plasma atomic emission spectrometer of the present invention
With following features：
1. establishing acidic flux melts zincizing agent sample-inductively coupled plasma atomic emission spectrometry to zincizing agent
The quick quantitative analytic method of middle Zn content；
2. measurement range：W (Zn) 20.00%~60.00%；
3. precision：
4. the plain standard liquid of special cell of the several elements consistent with matrix need not be used；And need not be numerous and diverse
Calibration curve solution, i.e. calibration curve is verbosely prepared to prepare simply；
5. the zincizing agent series standard material matched need not be difficult to.
Embodiment
The specific steps to the method for Zn content in measure zincizing agent involved in the present invention are described as follows below：
Step one：Sample is weighed
A ten thousandth electronic balance is used, 0.1000g zincizing agent samples is weighed, is placed in 50mL platinum crucibles；
Step 2：Pre-treatment melts
In the platinum crucible for being loaded with zincizing agent sample, about 2g potassium pyrosulfates are added, are mixed with thin wire；In high-temperature electric
Hinder in stove, be heated to 700 DEG C~750 DEG C melting samples, melt complete to sample；Take out, be placed on heat-resisting asbestos board, be cooled to
Room temperature；
Step 3：Melt leaches
Melt leaching includes the producing of water, the preparation of hydrochloric acid solution, the preparation of cosolvent solution and sample and dissolved；Ultra-pure water
Produce：Ultra-pure water is prepared using ultrapure water machine, the requirement of its electrical conductivity is not more than 0.10mS/m；The preparation of hydrochloric acid solution：In
In 400mL beakers, 200mL ultra-pure waters are added, 200mL hydrochloric acid is added, is stirred evenly with glass bar；Sample dissolves：In splendid attire melt
In platinum crucible, it is 20mL hydrochloric acid solutions (1+1) that fraction time, which adds total amount, and to leach melt, leaching test solution is transferred to 250mL beakers
In；Crucible is cleaned with ultra-pure water, washing lotion is incorporated in test solution；
Step 4：Test solution processing
Test solution processing is including boiling, cosolvent is prepared, cosolvent is added dropwise, test solution is cooled down.Boil：After melt is leached
Sample solution is heated to boiling.The preparation of 3% hydrogen peroxide cosolvent solution：In 250mL beakers, 20mL ultra-pure waters are added,
180mL30% hydrogen peroxide is added, is stirred evenly with glass bar；Cosolvent is added dropwise：In the 250mL for being loaded with sample solution boiled
In beaker, few drops of 3% hydrogen peroxide cosolvent solutions are added dropwise, continues to boil to solution and emits air pocket；Cool down test solution：It will help
Solvent handles and emits the companion 250mL of the test solution after air pocket beakers together, removes, is placed on heat-resisting asbestos board from electric furnace, cold
But to room temperature；
Step 5：Dilute constant volume
The sample solution of room temperature will be cooled to after sample dissolution process, be transferred in 100mL volumetric flasks, in transfer process
In, inserted with a glass bar in volumetric flask, tilt the beaker for containing sample solution, beaker is tight-lipped to lean on glass bar, makes solution edge
Glass bar is slowly flowed into, and glass bar lower end will be close to bottleneck inwall, but should not be too near to bottleneck, in order to avoid have solution spilling；Wait to try
After material solution flow to and do not flowed, beaker is carried slightly up along glass bar, while uprightly, making the drop solution stream for being attached to beaker oral area
It is back in beaker；The a little solution remained in beaker, with the washing 3~4 times of a small amount of two grades and above rank, cleaning solution is pressed
The above method is transferred in 100mL volumetric flasks；Sample solution is transferred to after volumetric flask completely, adds the water of two grades and above rank,
When being diluted to about 3/4 volume, volumetric flask yawing (is sure not to reverse and shaken) several times, makees preliminary mix；Then proceed to add two grades
And the water of above rank, during nearly graticule, be carefully added dropwise with dropper, until sample solution lower meniscus minimum point with
Untill graticule is tangent, glass stopper is covered tightly；
Left index finger pins glass stopper, and right hand finger tip withstands bottom of bottle edge, and volumetric flask the other way around and is shaken, then falls
Turn over, the bubble in solution is risen to top, so repeatedly 10 times~15 times, you can mix；
Step 6：Wavelength is selected
Inductively coupled plasma atomic emission spectrometer (ICP-AES) is opened, more than 2h is preheated；According to instrument specification
Instrument condition of work is optimized, suitable measuring condition is selected (when such as argon pressure, observed altitude, analytical line, flushing
Between, the time of integration, integral number of times etc.)；
Utilize Prodigy XP type inductively coupled plasma atomic emission spectrometers, the optimization measuring condition conduct of selection
Recommended work parameter；RF power：1100W；Argon gas input pressure：(85~95) PSI；Pump speed：1.0mL/min；Cooling gas flow：
20L/min；Secondary air amount：0.0L/min；Atomization gas flow：30PSI；Plasmatorch observed altitude：15mm；Sample injection time：
30s；The time of integration：10s；Purity of argon：It is not less than 99.99%；
Instrument condition of work optimization after, in element determination wavelength spectral line, according to Zn-ef ficiency content range, linear relationship,
The rate of recovery, testing result accuracy are considered, and selection is suitable to determine wavelength；Selected measure wavelength is：Zn
202.548nm、213.856nm；
Step 7：Zinc standard solution is prepared
1.0000g metallic zincs (>=99.9%) are dissolved by heating in 50mL salpeter solutions (1+1), moved into after cooling
In 100mL volumetric flasks, then add 50mL salpeter solutions (1+1), with two grades and the water of above rank, when being diluted to about 3/4 volume,
Volumetric flask yawing (is sure not to reverse and shaken) several times, makees preliminary mix；Then proceed to add the water of two grades and above rank, nearly mark
During line, carefully it is added dropwise with dropper, untill the minimum point and graticule of the lower meniscus of Zn-ef ficiency solution are tangent；Cover tightly
Glass stopper.Left index finger pins glass stopper, and right hand finger tip withstands bottom of bottle edge, and volumetric flask the other way around and is shaken, then
The other way around, the bubble in solution is risen to top, so repeatedly 10 times~15 times, mix；This is Zn-ef ficiency standard liquid
(1mL zinc containing 10mg)；
Step 8：It is prepared by calibration curve
In 6 50mL platinum crucibles, about 2g potassium pyrosulfates are separately added into, are mixed with thin wire；Same sample is operated below
Pre-treatment melting, melt leaching, sample dissolving；Be separately added into 0,2,3,4,5,6mL Zn-ef ficiency standard liquids, it is dilute with ultra-pure water
Release to scale, mix；
Step 9：ICP Atomic Emission Spectrometer AESs are detected
Click on plasmatorch to automatically begin to igniting, instrument operational factor is confirmed after igniting in normal range (NR), atomization system
System and plasma torch are working properly, more than stabilizer instrument 15min；
In on ICP Atomic Emission Spectrometer AESs, the spectral intensity of Zn-ef ficiency in solution to be measured is measured；Subtracted with each spectral intensity
Blank test solution spectrum intensity is net spectral intensity；Instrument reads the content ρ (Zn) of Zn-ef ficiency in solution to be measured automatically；
Step 10：The calculating of analysis result
According to the mass concentration of zinc in sample solution, represented with mg/mL, to calculate the mass fraction of zinc in zincizing agent；
Zn content is calculated in terms of mass fraction w (Zn) by formula (1) in zincizing agent sample：
In formula：
ρ (Zn) --- the numerical value of the mass concentration of zinc in test solution, unit is every milliliter of milligram (mg/mL)；
V --- the numerical value of test solution volume, unit is milliliter (mL)；
M --- the numerical value of sample quality, unit is gram (g)；
Step 11：Artificial synthesized standard specimen checking
(1) artificial synthesized standard specimen
The artificial synthesized standard specimen element addition of 5 kinds of zincizing agents is shown in Table 1；Synthetic standard sample nickeliferous 5%, alundum (Al2O3)
40%, appropriate ammonium fluoride etc.；After potassium pyrosulfate acidic flux melting etc. pre-treatment, it is transferred to water in 100mL volumetric flasks；
The artificial synthesized standard specimen element addition of table 1
| Numbering | Add nickel amount/mg | Add Al2O3Amount/mg | Add ammonium fluoride amount/mg | Add zinc amount/mg |
| 1# | 5.00 | 40 | In right amount | 20.00 |
| 2# | 5.00 | 40 | In right amount | 30.00 |
| 3# | 5.00 | 40 | In right amount | 40.00 |
| 4# | 5.00 | 40 | In right amount | 50.00 |
| 5# | 5.00 | 40 | In right amount | 60.00 |
(2) prepared by calibration curve
In 6 50mL platinum crucibles, about 2g potassium pyrosulfates are separately added into, are mixed with thin wire；Same sample is operated below
Pre-treatment melting, melt leaching, test solution processing etc.；Be separately added into 0,2.00,3.00,4.00,5.00,6.00mL Zn-ef ficiency marks
Quasi- solution, 100mL is diluted to ultra-pure water, is mixed；
(3) measure and calculate
Click on plasmatorch to automatically begin to igniting, instrument operational factor is confirmed after igniting in normal range (NR), atomization system
System and plasma torch are working properly, more than stabilizer instrument 15min；
In on ICP Atomic Emission Spectrometer AESs, the spectral intensity of Zn-ef ficiency in solution to be measured is measured；Subtracted with each spectral intensity
Blank test spectral intensity is net spectral intensity；Instrument reads the content ρ (Zn) of Zn-ef ficiency in solution to be measured automatically；By formula (1)
Calculate the mass fraction of zinc；
Synthetic standard sample evaluation is shown in Table 2；Illustrate this detection method measurement result accurately and reliably；
The synthetic standard sample evaluation of table 2
| Numbering | Element | Addition/mg | Content/% | Measurement result/% | Absolute difference/% | Tolerance/% | Conclusion |
| 1# | Zn | 20.00 | 20.00 | 20.18 | 0.18 | 0.35 | Meet the requirements |
| 2# | Zn | 30.00 | 30.00 | 29.78 | 0.22 | 0.40 | Meet the requirements |
| 3# | Zn | 40.00 | 40.00 | 40.39 | 0.39 | 0.45 | Meet the requirements |
| 4# | Zn | 50.00 | 50.00 | 50.43 | 0.43 | 0.50 | Meet the requirements |
| 5# | Zn | 60.00 | 60.00 | 59.53 | 0.47 | 0.50 | Meet the requirements |
Step 12：Production examination analysis result
Using a kind of ICP detection methods of Zn-ef ficiency content in zincizing agent, detection and precision have been carried out to material to be tested
Experiment, it produces examination analysis result referring to table 4；Its analysis result is accurately and reliably；
The production examination analysis result of table 4
| Numbering | Element | Measurement result w (Zn)/% | Average value/% | Standard deviation/% |
| 11# | Zn | 25.32 25.12 25.08 25.22 25.19 25.03 | 25.16 | 0.11 |
| 12# | Zn | 38.58 38.12 37.88 38.22 38.19 38.05 | 38.17 | 0.24 |
| 13# | Zn | 55.87 55.12 55.08 55.52 55.68 55.12 | 55.40 | 0.34 |
Claims (1)
1. a kind of method for determining Zn content in zincizing agent, it is characterized in that the step of this method is as follows：
Step one：Sample is weighed
A ten thousandth electronic balance is used, 0.1000g zincizing agent samples is weighed, is placed in 50mL platinum crucibles；
Step 2：Pre-treatment melts
In the platinum crucible for being loaded with zincizing agent sample, about 2g potassium pyrosulfates are added, are mixed with thin wire；In high temperature resistance furnace
In, 700 DEG C~750 DEG C melting samples are heated to, melt complete to sample；Take out, be placed on heat-resisting asbestos board, be cooled to room
Temperature；
Step 3：Melt leaches
Melt leaching includes the producing of water, the preparation of hydrochloric acid solution, the preparation of cosolvent solution and sample and dissolved；The system of ultra-pure water
Take：Ultra-pure water is prepared using ultrapure water machine, the requirement of its electrical conductivity is not more than 0.10mS/m；The preparation of hydrochloric acid solution：Burnt in 400mL
In cup, 200mL ultra-pure waters are added, 200mL hydrochloric acid is added, is stirred evenly with glass bar；Sample dissolves：In splendid attire melt platinum crucible
In, it is 20mL hydrochloric acid solutions (1+1) that fraction time, which adds total amount, and to leach melt, leaching test solution is transferred in 250mL beakers；With super
Pure water cleans crucible, and washing lotion is incorporated in test solution；
Step 4：Test solution processing
Test solution processing is including boiling, cosolvent is prepared, cosolvent is added dropwise, cooling test solution boils：Sample after melt is leached
Solution is heated to the preparation of 3% hydrogen peroxide cosolvent solution of boiling：In 250mL beakers, 20mL ultra-pure waters are added, are added
180mL30% hydrogen peroxide, is stirred evenly with glass bar；Cosolvent is added dropwise：In the 250mL beakers for being loaded with sample solution boiled
In, few drops of 3% hydrogen peroxide cosolvent solutions are added dropwise, continues to boil to solution and emits air pocket；Cool down test solution：By cosolvent
Handle and emit the companion 250mL of the test solution after air pocket beakers together, removed from electric furnace, be placed on heat-resisting asbestos board, be cooled to
Room temperature；
Step 5：Dilute constant volume
The sample solution of room temperature will be cooled to after sample dissolution process, be transferred in 100mL volumetric flasks, in transfer process, used
In a piece glass bar insertion volumetric flask, the beaker for containing sample solution is tilted, beaker is tight-lipped to lean on glass bar, makes solution along glass bar
Slowly flow into, glass bar lower end will be close to bottleneck inwall, but should not be too near to bottleneck, in order to avoid have solution spilling；Treat sample solution
It flow to after not flowing, beaker is carried slightly up along glass bar, while uprightly, makes the drop solution for being attached to beaker oral area flow back into burning
In cup；The a little solution remained in beaker, with the washing 3~4 times of a small amount of two grades and above rank, cleaning solution presses above-mentioned side
Method is transferred in 100mL volumetric flasks；Sample solution is transferred to after volumetric flask completely, is added the water of two grades and above rank, is diluted to
During about 3/4 volume, it is sure not to reverse and shakes by volumetric flask yawing several times, make preliminary mix；Then proceed to add two grades and with higher level
Other water, during nearly graticule, is carefully added dropwise with dropper, until the minimum point and graticule of the lower meniscus of sample solution are tangent
Untill, cover tightly glass stopper；
Left index finger pins glass stopper, and right hand finger tip withstands bottom of bottle edge, and volumetric flask the other way around and is shaken, then reversed
Come, the bubble in solution is risen to top, so repeatedly 10 times~15 times, you can mix；
Step 6：Wavelength is selected
Inductively coupled plasma atomic emission spectrometer (ICP-AES) is opened, more than 2h is preheated；According to instrument specification to instrument
Device condition of work is optimized, and selects suitable measuring condition, such as argon pressure, observed altitude, analytical line, washing time, product
Between timesharing, integral number of times etc.；
Using Prodigy XP type inductively coupled plasma atomic emission spectrometers, the optimization measuring condition of selection is used as recommendation
Running parameter；RF power：1100W；Argon gas input pressure：(85~95) PSI；Pump speed：1.0mL/min；Cooling gas flow：20L/
min；Secondary air amount：0.0L/min；Atomization gas flow：30PSI；Plasmatorch observed altitude：15mm；Sample injection time：30s；
The time of integration：10s；Purity of argon：It is not less than 99.99%；
After the optimization of instrument condition of work, in element determination wavelength spectral line, according to Zn-ef ficiency content range, linear relationship, recovery
Rate, testing result accuracy are considered, and selection is suitable to determine wavelength；Selected measure wavelength is：Zn
202.548nm、213.856nm；
Step 7：Zinc standard solution is prepared
1.0000g metallic zincs (>=99.9%) are dissolved by heating in 50mL salpeter solutions (1+1), 100mL is moved into after cooling and is held
In measuring bottle, then 50mL salpeter solutions (1+1) are added, with two grades and the water of above rank, when being diluted to about 3/4 volume, by capacity
Bottle yawing several times, is sure not to reverse and shaken, and makees preliminary mix；Then proceed to add the water of two grades and above rank, during nearly graticule, use
Dropper is carefully added dropwise, untill the minimum point and graticule of the lower meniscus of Zn-ef ficiency solution are tangent；Cover tightly glass stopper
Sub- left index finger pins glass stopper, and right hand finger tip withstands bottom of bottle edge, and volumetric flask the other way around and is shaken, then reversed
Come, the bubble in solution is risen to top, so repeatedly 10 times~15 times, mix；This is that (1mL contains Zn-ef ficiency standard liquid
10mg zinc)；
Step 8：It is prepared by calibration curve
In 6 50mL platinum crucibles, about 2g potassium pyrosulfates are separately added into, are mixed with thin wire；Operate below before same sample
Processing melts, melt leaches, sample dissolving；Be separately added into 0,2,3,4,5,6mL Zn-ef ficiency standard liquids, be diluted to ultra-pure water
Scale, is mixed；
Step 9：ICP Atomic Emission Spectrometer AESs are detected
Click on plasmatorch automatically begin to igniting, after igniting confirm instrument operational factor in normal range (NR), atomization system and
Plasma torch is working properly, more than stabilizer instrument 15min；
In on ICP Atomic Emission Spectrometer AESs, the spectral intensity of Zn-ef ficiency in solution to be measured is measured；Blank is subtracted with each spectral intensity
Testing liquid spectral intensity is net spectral intensity；Instrument reads the content ρ (Zn) of Zn-ef ficiency in solution to be measured automatically；
Step 10：The calculating of analysis result
According to the mass concentration of zinc in sample solution, represented with mg/mL, to calculate the mass fraction of zinc in zincizing agent；
Zn content is calculated in terms of mass fraction w (Zn) by formula (1) in zincizing agent sample：
In formula：
ρ (Zn) --- the numerical value of the mass concentration of zinc in test solution, unit is every milliliter of milligram (mg/mL)；
V --- the numerical value of test solution volume, unit is milliliter (mL)；
M --- the numerical value of sample quality, unit is gram (g)；
Step 11：Artificial synthesized standard specimen checking
(1) artificial synthesized standard specimen
The artificial synthesized standard specimen element addition of 5 kinds of zincizing agents is shown in Table 1；Synthetic standard sample nickeliferous 5%, alundum (Al2O3) 40%, are fitted
Measure ammonium fluoride etc.；After potassium pyrosulfate acidic flux melting etc. pre-treatment, it is transferred to water in 100mL volumetric flasks；
The artificial synthesized standard specimen element addition of table 1
(2) prepared by calibration curve
In 6 50mL platinum crucibles, about 2g potassium pyrosulfates are separately added into, are mixed with thin wire；Operate below before same sample
Processing is melted, melt leaches, test solution is handled etc.；Be separately added into 0,2.00,3.00,4.00,5.00,6.00mL Zn-ef ficiency standards it is molten
Liquid, 100mL is diluted to ultra-pure water, is mixed；
(3) measure and calculate
Click on plasmatorch automatically begin to igniting, after igniting confirm instrument operational factor in normal range (NR), atomization system and
Plasma torch is working properly, more than stabilizer instrument 15min；
In on ICP Atomic Emission Spectrometer AESs, the spectral intensity of Zn-ef ficiency in solution to be measured is measured；Blank is subtracted with each spectral intensity
Test spectrum intensity is net spectral intensity；Instrument reads the content ρ (Zn) of Zn-ef ficiency in solution to be measured automatically；Calculated by formula (1)
The mass fraction of zinc；
Synthetic standard sample evaluation is shown in Table 2；Illustrate this detection method measurement result accurately and reliably；
The synthetic standard sample evaluation of table 2
Step 12：Production examination analysis result
Using a kind of ICP detection methods of Zn-ef ficiency content in zincizing agent, detection and precision test have been carried out to material to be tested,
It produces examination analysis result referring to table 4；Its analysis result is accurately and reliably；
The production examination analysis result of table 4
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703120A (en) * | 2017-09-30 | 2018-02-16 | 重庆长安工业(集团)有限责任公司 | A kind of method of aluminium content in measure zincizing agent |
| CN107860762A (en) * | 2017-10-11 | 2018-03-30 | 重庆长安工业(集团)有限责任公司 | A kind of method of iron content in measure zincizing agent |
| CN108918508A (en) * | 2018-07-25 | 2018-11-30 | 重庆长安工业(集团)有限责任公司 | The measuring method of high content iron in a kind of tin bronze |
| CN109187505A (en) * | 2018-07-25 | 2019-01-11 | 重庆长安工业(集团)有限责任公司 | The measuring method of micro Zn content in tin bronze |
| CN113189088A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507484A (en) * | 2011-10-14 | 2012-06-20 | 济南康众医药科技开发有限公司 | Method for measuring content of zinc in compound montmorillonite preparation |
| CN102565025A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for measuring contents of aluminum, silicon and zinc in coating of aluminum-plated zinc plate |
| CN104280371A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial zinc oxide |
| CN106290317A (en) * | 2016-08-29 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | Potassium, lead and Direct spectrophotometry method in iron ore, slag and ion dust mud contaning |
-
2017
- 2017-04-24 CN CN201710271342.0A patent/CN106979945A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565025A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for measuring contents of aluminum, silicon and zinc in coating of aluminum-plated zinc plate |
| CN102507484A (en) * | 2011-10-14 | 2012-06-20 | 济南康众医药科技开发有限公司 | Method for measuring content of zinc in compound montmorillonite preparation |
| CN104280371A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial zinc oxide |
| CN106290317A (en) * | 2016-08-29 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | Potassium, lead and Direct spectrophotometry method in iron ore, slag and ion dust mud contaning |
Non-Patent Citations (2)
| Title |
|---|
| 李昌丽 等: "《火焰原子吸收光谱法测定红土镍矿中铜、锌、铬含量》", 《化学分析计量》 * |
| 胡建春 等: "《电解重量法和电感耦合等离子体原子发射光谱法在测定氧化镍中镍钴铜锌铁锰中的应用》", 《冶金分析》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703120A (en) * | 2017-09-30 | 2018-02-16 | 重庆长安工业(集团)有限责任公司 | A kind of method of aluminium content in measure zincizing agent |
| CN107860762A (en) * | 2017-10-11 | 2018-03-30 | 重庆长安工业(集团)有限责任公司 | A kind of method of iron content in measure zincizing agent |
| CN108918508A (en) * | 2018-07-25 | 2018-11-30 | 重庆长安工业(集团)有限责任公司 | The measuring method of high content iron in a kind of tin bronze |
| CN109187505A (en) * | 2018-07-25 | 2019-01-11 | 重庆长安工业(集团)有限责任公司 | The measuring method of micro Zn content in tin bronze |
| CN113189088A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
| CN113189088B (en) * | 2021-05-28 | 2022-09-06 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
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