CN110186743A - A kind of method that micro-wave digestion-ICP-AES quickly measures manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bi content in manganese iron simultaneously - Google Patents
A kind of method that micro-wave digestion-ICP-AES quickly measures manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bi content in manganese iron simultaneously Download PDFInfo
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- CN110186743A CN110186743A CN201810620119.7A CN201810620119A CN110186743A CN 110186743 A CN110186743 A CN 110186743A CN 201810620119 A CN201810620119 A CN 201810620119A CN 110186743 A CN110186743 A CN 110186743A
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Abstract
The present invention relates to a kind of methods that micro-wave digestion-ICP-AES quickly measures manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bi content in manganese iron simultaneously, using the automatic pre-treatment sample of micro-wave digestion, IEC data model is incorporated into calculation method with interference coefficient method, interference of the host element manganese to impurity elemental silicon, phosphorus, arsenic, lead, tin, antimony, bismuth can be effectively rationally sheltered using interference coefficient method correction in ICP spectrometer, realizes Major And Minor Elements Synchronization Analysis.The sample of the application is converted to liquid under high-pressure sealed state, can avoid the loss of trace element arsenic, lead, tin, antimony, bismuth to the maximum extent, improves the accuracy of analysis result, only uses HCl and HNO in digestion process3, usage amount is few, pollution and cost is preferably minimized, more clean and environmental protection.
Description
Technical field
The invention belongs to metallurgical analysis technical fields, and in particular to it is a kind of quickly measure simultaneously manganese in manganese iron, silicon, phosphorus, arsenic,
The detection method of lead, tin, antimony, bi content.
Background technique
Manganeisen manganese content 70%~85%, iron 10%~30%, remaining is low content impurity.By phosphorus content height point
For high carbon ferromanganese, mid-carbon fe-mn, low-carbon ferromanganese etc..Manganese iron is a kind of alloy material as steel-making one of most important deoxidier
Material, can both play deoxidation, main amount manganese element therein is also alloy addition, can be effectively improved finished product in smelting process
The quality and mechanical performance of steel.But impurity component such as arsenic, lead, tin, antimony, the bismuth in manganeisen can not be gone in smelting process
Remove, finished steel will be brought directly to, these low content impurities influence the performances of steel very big, it is necessary to be strict controlled in 5ppm with
It is interior.Therefore manganese iron must be strictly controlled its impurity content as the deoxidier and alloy addition of steel-making.
Host element manganese in manganese iron is at present according to GB/T5686.1-2008 perchloric acid oxidation's titration, method accuracy
Height, but process is cumbersome, and detection cycle is longer.Detection for impurity element in manganese iron, mainly has: the steel community of stock of Inner Mongol Baogang
Part Co., Ltd measures Silicon in Ferromanganese phosphorus content using inductively coupled plasma spectrometry transmitter, and the method pre-treatment is excessively
It is cumbersome and two kinds of elements can only be analyzed；A kind of stability and high efficiency, sensitive and accurate has been invented by Kunming Iron And Steel Co., Ltd, Wuhan Iron and Steel Plant group
Chromium in manganese iron, tin, arsenic content detection method, agents useful for same is related to hydrofluoric acid and perchloric acid in the method, belongs to danger
Chemicals, and both acid easily causeTin and arsenicLoss；Also periodical report surveys using MTG YBCO bulk-X fluorescence spectrum method
Determine Silicon in Ferromanganese, manganese, phosphorus, chromium, nickel, copper, this method needs platinum crucible to melt during the experiment, after high-volume melts sample,
Platinum crucible can be lost causes sheet glass difficulty demoulding need to polish again, improve analysis cost, and do not analyze harmful element arsenic,
Lead, tin, antimony, bi content；Angang Stock Co., Ltd technique center is using in inductively coupled plasma mass spectrometry measurement manganese iron
Trace Lead and Tin antimony, the method use hydrochloric acid+nitric acid+hydrofluoric acid+perchloric acid+hydrogen peroxide decomposition samples, acid system mistake used
It is more and to be related to hazardous chemical less environmentally friendly, furthermore it is unfavorable to the analysis of Determination of Trace Amounts of Lead, Tin antimony that open type acid is molten.
In conclusion there has been no one kind not only can analyze host element manganese in manganese iron at present, but also manganese iron can be analyzed comprehensively
The method generation of middle silicon, phosphorus, arsenic, lead, tin, antimony, bi content.
Summary of the invention
That the purpose of the present invention is to provide a kind of sample pretreatings is simple and environmentally-friendly, host element in the quick manganeisen of measurement
The detection method of manganese and impurity elemental silicon, phosphorus, arsenic, lead, tin, antimony, bi content mentions more particularly to avoid the loss of trace element
The precision of high detection.
The present invention solves the above problems used technical solution are as follows: a kind of micro-wave digestion-ICP-AES is quickly measured simultaneously
The method of manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bi content in manganese iron, steps are as follows
(1) closed Microwave assisted sample digestion: accurately weighing sample, be accurate to 0.1mg, is placed in TFM counteracting tank, is put into
In HTC safety guard, is soaked with a small amount of ultrapure water, sequentially adds hydrochloric acid and nitric acid, gently shake solution, run out of portion gas,
TFM lid and safety spring piece are covered, tightens lid with torque spanner, is put into resolution instrument and is cleared up；After clearing up EP (end of program),
30 DEG C are cooled to hereinafter, digestion solution is transferred in volumetric flask, inner cover is cleaned multiple times on a small quantity with ultrapure water and clears up inner canister, washing lotion
Merging is transferred in volumetric flask, is settled to scale with ultrapure water, is shaken up, and is stood, is prepared into prepare liquid；
(2) standard solution is prepared: weighing a certain amount of high-purity manganese and 6 parts of high purity iron are respectively placed in 6 beakers, sequentially add
Hydrochloric acid and nitric acid dissolve by heating on electric hot plate, removed after the clarification of manganese iron matrix sample it is cooling after it is spare, take 6 volumetric flasks,
Silicon, copper, phosphorus, arsenic, lead, tin, antimony, bismuth series standard solution are sequentially added, the iron-based liquid solution of manganese after cooling is added, with ultrapure water
It is diluted to scale, is mixed；
(3) ICP spectroscopic assay: ICP measuring instrument is opened, meets the requirements and lights a fire stable half an hour to each index of instrument
Afterwards, the analysis method that sample is established according to the operating condition of ICP, optimizes the pressure of two pump folders, while IEC is established in method
Data model is successively incorporated into the interference coefficient K value of each detection elements, in order sequentially determining blank solution, standard solution and to
Survey liquid, using concentration value as abscissa, intensity value be ordinate linear curve, calculate manganese iron in manganese, silicon, phosphorus, arsenic, lead, tin,
Antimony, bismuth element content.
Preferably, in step (1) by taking 0.2000g sample as an example, the dosage of hydrochloric acid and nitric acid is 10mL hydrochloric acid+5mL nitric acid；
The dosage of hydrochloric acid used in manganese dissolved ferric iron and nitric acid is 10mL hydrochloric acid+5mL nitric acid in step (2).
Specifically, the concrete operations of step (1) are to accurately weigh sample 0.2000g, are accurate to 0.1mg, are placed in TFM and disappear
It solves in tank, is put into HTC safety guard, soaked with a small amount of ultrapure water, sequentially add 10mL hydrochloric acid and 5mL nitric acid, gently shake molten
Liquid runs out of its portion gas, continues 5-10 minutes, covers TFM lid and safety spring piece, tightens lid with torque spanner, puts
Enter in microwave cavity, connect temperature sensor, while in company with blank sample is prepared, being put into microwave dissolver and being cleared up, being disappeared
After solving EP (end of program), it is cooled to 30 DEG C hereinafter, digestion solution is transferred in 100mL quartz volumetric flask, it is multiple on a small quantity with ultrapure water
Inner cover and resolution inner canister are cleaned, washing lotion merging is transferred in quartzy volumetric flask, is settled to scale with ultrapure water, shakes up, stands, system
For at prepare liquid.
Preferably, step (1) micro-wave digestion condition is, power 600W~800W, pressure 800psi, time-to-climb are cleared up
20min or more, retention time 25min or more, 220 ± 20 DEG C of temperature.When clearing up sample quantities no more than 4, power is cleared up
600W can be reduced to, remaining parameter constant.
The configuration of step (2) calibration curve solution: high-purity manganese sample weighting amount (g) are as follows: 0,0.10,0.12,0.14,0.16,
0.18；6 parts of sample weighting amount of high purity iron are 0.0200g, and the mass concentration (μ g/mL) of each element of mixed standard solution is respectively
Are as follows: Si:0,2,10,20,30,40；P:0,1,2,4,6,8；As, Pb, Sn, Sb, Bi are equal are as follows: 0,0.04,0.1,0.2,0.4,
0.6；It is respectively Mn:0,50,60,70,80,90 that all constituent contents to be measured, which are converted into mass fraction content (%),；Si:0,
0.1,0.5,1.0,1.5,2.0；P:0,0.05,0.1,0.2,0.3,0.4；As, Pb, Sn, Sb, Bi are equal are as follows: 0,0.002,
0.005、0.01、0.02、0.03。
Preferably, inductive coupling plasma emission spectrograph operating condition is specifically, RF power in step (3):
1150W, secondary air: 0.5L/min, nebulizer gas flow: 0.7L/min, cooling gas flow: 12L/min, pump speed is rinsed
100rpm, analysis pump speed 50rpm.
The application is mainly the interference that eliminate Main elements Mn to the especially trace element of other measurement elements,
The interference of each measurement element, interference coefficient K of the Main elements Mn to Si, P, As, Pb, Sn, Sb, Bi are incorporated into IEC data model
Value is respectively as follows: 0.00023,0.036,0.011,0.0089,0.034,0.021,0.019.The corresponding analysis spectral line of each element are as follows:
Mn-403.076nm、Si-251.611nm、P-178.284nm、As-189.042nm、Pb-220.353nm、Sn-189.989nm、
Sb-206.833nm、Bi-223.061nm。
Compared with the prior art, the advantages of the present invention are as follows:
(1) it is incorporated into IEC data model in method foundation with interference coefficient method, rationally utilizes interference system in ICP spectrometer
Number method correction can effectively shelter interference of the host element manganese to impurity elemental silicon, phosphorus, arsenic, lead, tin, antimony, bismuth, realize that Major And Minor Elements are same
Step analysis embodies intelligence instrument and gradually replaces manual operation, can make up deficiency in the prior art.
(2) ICP spectrometer is utilized, optimized analysis spectral line is selected, runs calibration curve, can quickly be determined high in experiment
The content of manganese and other multiple object elements.
(3) sample of the application is converted to liquid under high-pressure sealed state, can avoid to the maximum extent trace element arsenic,
Lead, tin, antimony, bismuth loss, improve the accuracy of analysis result.
(4) agents useful for same of the present invention only hydrochloric acid and nitric acid, avoids using hazardous chemical used in traditional experiment, such as hydrogen fluorine
Acid and perchloric acid etc. endanger experiment operator and reduce；For 0.2g sample, sour total amount only discharge after testing by 15mL, end
Waste acid quantity very little, less pollution are more environmentally-friendly.
Specific embodiment
Present invention is further described in detail with reference to embodiments.
A kind of micro-wave digestion-ICP-AES of the invention quickly measures manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bismuth in manganese iron simultaneously
The method of content.
Test device therefor: U.S. Thermo Fisher6500Duo composes direct-reading inductively coupled plasma atomic emission entirely
Instrument；U.S. CE M Mars6 microwave dissolver；German Sai Duolisi electronic balance
Test agents useful for same: hydrochloric acid (excellent pure grade)；Nitric acid (excellent pure grade)；Ultrapure water (self-control)；Standard reserving solution: Si, P,
The Standard Stock solutions of As, Pb, Sn, Sb, Bi are provided by national Iron and Steel Research Geueral Institute, except the concentration value of Si, Sn and Sb are 500
Outside μ g/mL, the concentration value of remaining standard solution is 1000 μ g/mL；Primary standard substance: high-purity manganese (manganese mass fraction 99.91%)；
High purity iron (weight of iron score 99.98%).
For the accuracy for verifying the method for the present invention measurement result, the high-carbon of the number YSBC11602-99 of known content is chosen
Manganese iron standard sample is as example 1, and BH0304-8 mid-carbon fe-mn standard sample is as example 2, GSB03-1316-2000 low Carbon Manganese
Iron standard sample is as example 3, and GSB03-1797-2005 nitrided ferromanganese standard sample is as example 4.
Manganese in the manganese iron standard sample of example 1~4, silicon, phosphorus, arsenic, lead, tin, antimony, bismuth element measuring method include following
Step:
(1) sample decomposes: accurately weighing sample 0.2000g, is accurate to 0.1mg, be placed in TFM counteracting tank, is put into HTC peace
It in full cover, is soaked with a small amount of ultrapure water, sequentially adds 10mL hydrochloric acid and 5mL nitric acid, gently shake solution, run its portion gas
(5-10 minutes) out, cover TFM lid and safety spring piece, tighten lid with torque spanner, are put into microwave cavity, connect temperature
Sensor, while in company with blank sample is prepared, it is put into microwave dissolver and is cleared up by 1 program of table.After clearing up EP (end of program),
30 DEG C are cooled to hereinafter, digestion solution is transferred in 100mL quartz volumetric flask, inner cover and resolution are cleaned multiple times on a small quantity with ultrapure water
Inner canister, washing lotion merging are transferred in quartzy volumetric flask, are settled to scale with ultrapure water, shake up, stand, be prepared into prepare liquid.
1 micro-wave digestion program of table
| Step | Time (min) | Power (W) | Temperature (DEG C) | Pressure (psi) |
| 1 | 20 | 800 | 220 | 800 |
| 2 | 25 | 800 | 220 | 800 |
(2) standard solution working curve prepare: take 6 250mL beakers, weigh respectively 0g, 0.10g, 0.12g, 0.14g,
The high-purity manganese of 0.16g, 0.18g and 0.0200g high purity iron sequentially add 10mL hydrochloric acid and 5mL nitric acid in electric heating in this 6 beakers
It dissolves by heating, is removed after the clarification of matrix sample spare after cooling down on plate.Take 6 100mL volumetric flasks, sequentially add silicon, copper,
Phosphorus, arsenic, lead, tin, antimony, bismuth series standard solution, are added the iron-based liquid solution of manganese after cooling, wherein for only in the 1st volumetric flask
Containing iron-based and reagent blank, scale is diluted to ultrapure water, is mixed.Each element content is shown in Table 2 in standard curve.
Each element mass fraction content (%) in 2 calibration curve solution of table
| Element | Standard 1 | Standard 2 | Standard 3 | Standard 4 | Standard 5 |
| Mn | 50 | 60 | 70 | 80 | 90 |
| Si | 0.1 | 0.5 | 1.0 | 1.5 | 2.0 |
| P | 0.05 | 0.1 | 0.2 | 0.3 | 0.4 |
| As | 0.002 | 0.005 | 0.010 | 0.020 | 0.030 |
| Pb | 0.002 | 0.005 | 0.010 | 0.020 | 0.030 |
| Sn | 0.002 | 0.005 | 0.010 | 0.020 | 0.030 |
| Sb | 0.002 | 0.005 | 0.010 | 0.020 | 0.030 |
| Bi | 0.002 | 0.005 | 0.010 | 0.020 | 0.030 |
Eight element measurement of ICP: optimization instrument parameter makes instrument be in optimum state: RF power: 1150W, secondary air:
0.5L/min, nebulizer gas flow: 0.7L/min, cooling gas flow: 12L/min, pump speed 100rpm, analysis pump speed are rinsed
50rpm chooses Mn-403.076nm, Si-251.611nm, P-178.284nm, As-189.042nm, Pb-220.353nm, Sn-
189.989nm,Sb-206.833nm,Bi-223.061nm.Internal standard element Ar wavelength: 404.442nm.Calculate Mn to Si, P,
The interference coefficient K value of As, Pb, Sn, Sb, Bi, respectively 0.00023,0.036,0.011,0.0089,0.034,0.021,
0.019, and K value is incorporated into IEC data model method for building up.Sequentially determining blank solution, standard solution and prepare liquid in order,
Using concentration value as abscissa, intensity value is ordinate linear curve, calculates manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bismuth in manganese iron
Constituent content.
Linear relationship and detection limit: the related coefficient of each element is respectively Mn, Si, P, As, Pb, Sn, Sb, Bi:
0.9999,0.9999,0.9992,0.9994,0.9991,0.9990,0.9989,0.9987；Detection limit (%) Mn, Si, P, As,
Pb, Sn, Sb, Bi:0.022,0.0064,0.0050,0.0005,0.0002,0.0003,0.0001,0.0001.
Detection structure is referring to table 3.
3 preci-sion and accuracy of table (n=8) %
| Element | Mn | Si | P | As | Pb | Sn | Sb | Bi |
| Standard value 1 | 73.88 | 0.43 | 0.152 | 0.0082 | 0.0002 | 0.0017 | 0.0007 | < 0.0001 |
| Example 1 | 73.72 | 0.441 | 0.150 | 0.0081 | 0.0002 | 0.0018 | 0.0005 | < 0.0001 |
| RSD | 0.89 | 1.11 | 2.34 | 5.02 | 9.11 | 6.05 | 8.89 | 9.18 |
| Standard value 2 | 79.44 | 1.51 | 0.344 | 0.0088 | 0.0032 | 0.0002 | 0.0005 | < 0.0001 |
| Example 2 | 79.51 | 1.488 | 0.341 | 0.0089 | 0.0030 | 0.0002 | 0.0003 | < 0.0001 |
| RSD | 0.92 | 1.06 | 1.89 | 5.22 | 6.02 | 9.88 | 9.62 | 10.14 |
| Standard value 3 | 84.28 | 0.62 | 0.196 | 0.0037 | 0.0010 | 0.0010 | 0.0005 | < 0.0001 |
| Example 3 | 84.08 | 0.614 | 0.201 | 0.0037 | 0.0009 | 0.0011 | 0.0005 | < 0.0001 |
| RSD | 1.01 | 2.29 | 2.56 | 5.68 | 9.75 | 10.10 | 10.31 | 10.50 |
| Standard value 4 | 74.02 | 1.70 | 0.183 | 0.0382 | 0.0044 | 0.0006 | 0.0021 | < 0.0001 |
| Example 4 | 74.16 | 1.688 | 0.185 | 0.0384 | 0.0040 | 0.0005 | 0.0020 | < 0.0001 |
| RSD | 0.86 | 1.41 | 2.96 | 4.86 | 7.23 | 10.0 | 8.96 | 11.21 |
Note: As, Pb, Sn, Sb, Bi content are not marked in the manganese iron standard sample in example 1~4, this data is by Beijing steel
Iron research institute provides.
From testing result as can be seen that the constituent content detected using the application detection method is compared with standard content,
It is very close, precise measurement is carried out more particularly to the content to trace element As, Pb, Sn, Sb, it is consistent with standard value to measure value,
Test result shows that the application can effectively avoid the loss of element, eliminates influence of the main amount manganese to other elements assay.
The Applicant declares that the present invention illustrates detection method process of the invention by examples detailed above, but the present invention is not
It is confined to aforesaid operations step, that is, does not mean that the present invention must rely on aforesaid operations process and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, adds reagent equivalence replacement and analytical element used in the present invention
Add, all of which fall within the scope of protection and disclosure of the present invention.
Claims (8)
1. the side that a kind of micro-wave digestion-ICP-AES quickly measures manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bi content in manganese iron simultaneously
Method, it is characterised in that: steps are as follows
(1) closed Microwave assisted sample digestion: accurately weighing sample, be accurate to 0.1mg, is placed in TFM counteracting tank, is put into HTC peace
In full cover, is soaked with a small amount of ultrapure water, sequentially add hydrochloric acid and nitric acid, gently shake solution, run out of portion gas, cover
TFM lid and safety spring piece tighten lid with torque spanner, are put into resolution instrument and are cleared up；It is cooling after clearing up EP (end of program)
To 30 DEG C hereinafter, digestion solution is transferred in volumetric flask, inner cover and resolution inner canister is cleaned multiple times on a small quantity with ultrapure water, washing lotion merges
It is transferred in volumetric flask, is settled to scale with ultrapure water, shakes up, stand, be prepared into prepare liquid；
(2) standard solution is prepared: weighing a certain amount of high-purity manganese and 6 parts of high purity iron are respectively placed in 6 beakers, sequentially add hydrochloric acid
Dissolved by heating on electric hot plate with nitric acid, removed after the clarification of manganese iron matrix sample it is cooling after it is spare, take 6 volumetric flasks, successively
Silicon, copper, phosphorus, arsenic, lead, tin, antimony, bismuth series standard solution is added, the iron-based liquid solution of manganese after cooling is added, is diluted with ultrapure water
To scale, mix；
(3) ICP spectroscopic assay: opening ICP measuring instrument, meet the requirements after each index of instrument and after stable half an hour of lighting a fire, according to
The analysis method that sample is established according to the operating condition of ICP, optimizes the pressure of two pump folders, while IEC data are established in method
Model is successively incorporated into the interference coefficient K value of each detection elements, in order sequentially determining blank solution, standard solution and prepare liquid,
Using concentration value as abscissa, intensity value is ordinate linear curve, calculates manganese, silicon, phosphorus, arsenic, lead, tin, antimony, bismuth in manganese iron
Constituent content.
2. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: in step (1) by taking 0.2000g sample as an example, the dosage of hydrochloric acid and nitric acid is 10mL
Hydrochloric acid+5mL nitric acid；The dosage of hydrochloric acid used in manganese dissolved ferric iron and nitric acid is 10mL hydrochloric acid+5mL nitric acid in step (2).
3. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: the concrete operations of step (1) are to accurately weigh sample 0.2000g, are accurate to
0.1mg is placed in TFM counteracting tank, is put into HTC safety guard, is soaked with a small amount of ultrapure water, is sequentially added 10mL hydrochloric acid and 5mL
Nitric acid gently shakes solution, runs out of its portion gas, continues 5-10 minutes, covers TFM lid and safety spring piece, uses torque
Spanner tightens lid, is put into microwave cavity, connects temperature sensor, while in company with blank sample is prepared, being put into micro-wave digestion
It is cleared up in instrument, after clearing up EP (end of program), is cooled to 30 DEG C hereinafter, digestion solution is transferred in 100mL quartz volumetric flask, use
Inner cover and resolution inner canister is cleaned multiple times in ultrapure water on a small quantity, and washing lotion merging is transferred in quartzy volumetric flask, is settled to quarter with ultrapure water
Degree, shakes up, and stands, is prepared into prepare liquid.
4. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: step (1) micro-wave digestion condition is to clear up power 600W~800W, pressure
800psi, time-to-climb 20min or more, retention time 25min or more, 220 ± 20 DEG C of temperature.
5. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: high-purity manganese sample weighting amount (g) in step (2) are as follows: 0,0.10,0.12,0.14,0.16,
0.18；6 parts of sample weighting amount of high purity iron are 0.0200g, and the mass concentration (μ g/mL) of each element of mixed standard solution is respectively
Are as follows: Si:0,2,10,20,30,40；P:0,1,2,4,6,8；As, Pb, Sn, Sb, Bi are equal are as follows: 0,0.04,0.1,0.2,0.4,
0.6；It is respectively Mn:0,50,60,70,80,90 that all constituent contents to be measured, which are converted into mass fraction content (%),；Si:0,
0.1,0.5,1.0,1.5,2.0；P:0,0.05,0.1,0.2,0.3,0.4；As, Pb, Sn, Sb, Bi are equal are as follows: 0,0.002,
0.005、0.01、0.02、0.03。
6. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: inductive coupling plasma emission spectrograph operating condition in step (3) specifically,
RF power: 1150W, secondary air: 0.5L/min, nebulizer gas flow: 0.7L/min, cooling gas flow: 12L/min, punching
Wash pump speed 100rpm, analysis pump speed 50rpm.
7. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: Main elements Mn distinguishes the interference coefficient K value of Si, P, As, Pb, Sn, Sb, Bi
Are as follows: 0.00023,0.036,0.011,0.0089,0.034,0.021,0.019.
8. micro-wave digestion-ICP-AES according to claim 1 quickly simultaneously measure manganese in manganese iron, silicon, phosphorus, arsenic, lead, tin,
The method of antimony, bi content, it is characterised in that: the analysis spectral line of each element in step (3) are as follows: Mn-403.076nm, Si-
251.611nm、P-178.284nm、As-189.042nm、Pb-220.353nm、Sn-189.989nm、Sb-206.833nm、Bi-
223.061nm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964698A (en) * | 2021-02-22 | 2021-06-15 | 青岛斯坦德检测股份有限公司 | Method for measuring high-content tin in copper alloy by ICP-OES |
| CN113720828A (en) * | 2021-09-27 | 2021-11-30 | 江苏省地质工程勘察院 | Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
| CN114199645A (en) * | 2021-12-09 | 2022-03-18 | 浙江浙能技术研究院有限公司 | Method for analyzing magnesium, aluminum, iron and silicon in gypsum slurry by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) |
| CN115308012A (en) * | 2022-08-31 | 2022-11-08 | 中国科学院地球化学研究所 | Pretreatment method for measuring antimony isotope in water with low antimony content |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105987896A (en) * | 2016-05-24 | 2016-10-05 | 江苏泰富兴澄特殊钢有限公司 | Method for rapidly and simultaneously determining content of six elements in chromite by microwave digestion-ICP (Inductively Coupled Plasma)-AES (Atomic Emission Spectroscopy) |
| CN106290311A (en) * | 2016-07-21 | 2017-01-04 | 江苏泰富兴澄特殊钢有限公司 | A kind of micro-wave digestion ICP AES measures the method for ten kinds of constituent contents in 70 ferrotianiums the most simultaneously |
| KR101716451B1 (en) * | 2015-05-07 | 2017-03-14 | 이상익 | System for detail analysis of powder with metal foreign substance |
-
2018
- 2018-06-15 CN CN201810620119.7A patent/CN110186743A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101716451B1 (en) * | 2015-05-07 | 2017-03-14 | 이상익 | System for detail analysis of powder with metal foreign substance |
| CN105987896A (en) * | 2016-05-24 | 2016-10-05 | 江苏泰富兴澄特殊钢有限公司 | Method for rapidly and simultaneously determining content of six elements in chromite by microwave digestion-ICP (Inductively Coupled Plasma)-AES (Atomic Emission Spectroscopy) |
| CN106290311A (en) * | 2016-07-21 | 2017-01-04 | 江苏泰富兴澄特殊钢有限公司 | A kind of micro-wave digestion ICP AES measures the method for ten kinds of constituent contents in 70 ferrotianiums the most simultaneously |
Non-Patent Citations (3)
| Title |
|---|
| 张艳 等: "高碳锰铁中微量元素含量的快速测定", 《金属制品》 * |
| 李成福 等: "微波消解—电感耦合等离子体原子发射光谱法快速测定汉中天台山锰矿中二氧化硅含量", 《中国锰业》 * |
| 许春向 等: "《现代卫生化学》", 29 February 2000, 人民卫生出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964698A (en) * | 2021-02-22 | 2021-06-15 | 青岛斯坦德检测股份有限公司 | Method for measuring high-content tin in copper alloy by ICP-OES |
| CN113720828A (en) * | 2021-09-27 | 2021-11-30 | 江苏省地质工程勘察院 | Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
| CN114199645A (en) * | 2021-12-09 | 2022-03-18 | 浙江浙能技术研究院有限公司 | Method for analyzing magnesium, aluminum, iron and silicon in gypsum slurry by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) |
| CN114199645B (en) * | 2021-12-09 | 2024-04-16 | 浙江浙能技术研究院有限公司 | Method for analyzing magnesium, aluminum, iron and silicon in gypsum slurry by microwave digestion-ICP-AES |
| CN115308012A (en) * | 2022-08-31 | 2022-11-08 | 中国科学院地球化学研究所 | Pretreatment method for measuring antimony isotope in water with low antimony content |
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