CN111751298A - Method for measuring content of non-metal elements in crude lead - Google Patents
Method for measuring content of non-metal elements in crude lead Download PDFInfo
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- CN111751298A CN111751298A CN202010714624.5A CN202010714624A CN111751298A CN 111751298 A CN111751298 A CN 111751298A CN 202010714624 A CN202010714624 A CN 202010714624A CN 111751298 A CN111751298 A CN 111751298A
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910052755 nonmetal Inorganic materials 0.000 title claims description 11
- 238000001514 detection method Methods 0.000 claims abstract description 40
- 239000002893 slag Substances 0.000 claims abstract description 31
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004448 titration Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims description 12
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000956 alloy Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910000464 lead oxide Inorganic materials 0.000 description 3
- 229940056932 lead sulfide Drugs 0.000 description 3
- 229910052981 lead sulfide Inorganic materials 0.000 description 3
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007974 sodium acetate buffer Substances 0.000 description 2
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention relates to the technical field of lead-based alloy detection, in particular to a method for determining the content of non-metallic elements in lead bullion, wherein the content of the non-metallic elements in the lead bullion is directly related to lead-containing slag, and the method mainly solves the problems that the detection precision is poor and the detection result is easy to diverge when the lead bullion and the lead-containing slag are determined in a rough manner and the determination standard is not uniform. The determination method comprises two times of lead content detection of electrolytic lead and crude lead, namely direct-reading spectrometer detection and EDTA titration detection, and the content of non-metallic elements is calculated by analyzing the difference value of the two times of detection, so that the lead slag of the crude lead is represented. The method provided by the invention indirectly calculates the content of the non-metallic elements which are difficult to directly measure by two detection methods with different principles, and has the advantages of simple principle and high detection precision.
Description
Technical Field
The invention belongs to the technical field of lead-based alloy detection, and particularly relates to a method for determining the content of non-metal elements in crude lead.
Background
Lead produced after the lead-containing material is smelted by the smelting furnace is lead bullion. In the smelting process, non-metallic elements (mainly oxygen and sulfur) which are not completely reacted in a small amount of lead-containing materials are combined with the crude lead to form substances such as lead oxide, lead sulfide and the like. Because the temperature is high (more than 800 ℃) in the lead discharging process, lead oxide, lead sulfide and the like are dissolved in the crude lead and discharged together with the crude lead. During the slagging process of the crude lead, the temperature is low (about 400 ℃), lead oxide, lead sulfide and the like are separated from the crude lead and float to the surface of lead liquid to form pasty slag. Slag removing agent is added to produce dry slag, which is lead-containing slag of the crude lead and needs to be fished out from the surface of the lead liquid.
Therefore, the lead-containing slag of the crude lead determines the quality of the crude lead and the operation amount of the crude lead refining process, and is an important index for representing the quality of the crude lead. In the process of making dry slag, the slag making temperature, the components and the adding amount of a slag removing agent and the stirring working condition all have certain influence on the dry slag amount, so that the problems of low detection precision of lead contained slag and easy divergence of detection results are caused.
Disclosure of Invention
The invention aims to provide a reliable method for detecting non-metal elements in lead bullion, which is used for representing the slag content of lead bullion and solves the problems that the detection precision of the slag content of lead bullion is low and the detection result is easy to diverge in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme that the method for measuring the non-metal elements in the crude lead comprises the following steps:
a. preparing an electrolytic lead sample, detecting by a direct-reading spectrometer, and recording the detection result as W1The electrolytic lead sample is detected by an EDTA titration method, and the detection result is recorded as w1；
b. Preparing a crude lead and lead ingot sample, and recording a detection result as W by a direct-reading spectrometer2The crude lead ingot sample is detected by EDTA titration method, and the detection result is recorded as w2；
c. The filtration coefficient a of the electrolytic lead is calculated according to the following formula:
a＝w1/W1；
d. correcting the lead bullion content w detected by EDTA titration by using the filtering coefficient a in the step c2Thereby obtaining the real lead content W of the crude leadPb(ii) a And then the content W of the lead bullion detected by a direct-reading spectrometer2Minus the true lead content WPbObtaining the content W of the non-metallic elementsOAnd characterizing the lead containing slag W of the lead bullion accordinglySlag. The true lead content WPbThe value is the crude lead content w of EDTA determination after the filtration coefficient a correction2I.e. WPb＝w2A, the content of said non-metallic element WOOf value WO＝W2－w2A; the lead bullion containing slag WSlagOf value WSlagCan be estimated to be 9.63WO。
Preferably, step a or b comprises the following steps: 1. taking a crude lead ingot sample, putting the crude lead ingot sample into a beaker, digesting the crude lead ingot sample by nitric acid, and steaming the crude lead ingot sample until the crude lead ingot sample is nearly dry; 2. adding sulfuric acid, continuously steaming until a large amount of white smoke is emitted, stopping heating, and cooling; 3. Adding distilled water along the wall of the cup, boiling, and cooling; 4. filtering with filter paper, washing the precipitate with distilled water, and transferring the filter paper and the precipitate into an original beaker; 5. washing the wall of the cup with distilled water, adding acetic acid-sodium acetate buffer solution, heating to boil, dripping 1-2 drops of xylenol orange indicator, and titrating with a calibrated EDTA standard solution until the solution fades from red and then turns into bright yellow as a terminal point; 6. and reading the consumption of the EDTA standard solution, and calculating the lead content of the lead bullion.
The principle of the technical scheme of the invention is as follows:
1. recording the content of other metal elements in the lead ingot as WMeTrue lead content of WPbW as a non-metallic elementOThe method comprises the following steps: wPb+WMe+WO1 is ═ 1; the lead content measured by the direct-reading spectrometer is the balance;
and 2, recording the lead content of the spectrum detection as W, wherein the lead content comprises the following components: w is 1-WMe＝WPb+WO；
3. The lead content w determined by the EDTA titration method is corrected by the filter coefficient a to obtain the real lead content, which comprises the following steps: wPb＝w/a；
4. The content W of the non-metallic element can be calculated by measuring the content W of lead by W, EDTA titration method of the lead content detected by spectrumONamely:W－w/a＝WPb+WO－WPb＝WO(ii) a The lead content results of electrolytic lead and crude lead are detected by respectively using a direct-reading spectrometer and an EDTA titration method, so that the content of non-metal elements in the crude lead can be calculated, and the lead slag of the crude lead is represented.
The invention has the beneficial effects that: the invention mainly solves the problems that the detection precision is poor and the detection results are easy to diverge when multi-party detection is involved due to the fact that the crude lead and lead containing slag has rough detection modes and non-uniform detection standards. The determination method comprises two times of lead content detection of electrolytic lead and crude lead, namely direct-reading spectrometer detection and EDTA titration detection, and the content of non-metallic elements is calculated by analyzing the difference value of the two times of detection, so that the lead slag of the crude lead is represented. The method provided by the invention indirectly calculates the content of the non-metallic elements which are difficult to directly measure by two detection methods with different principles, and has the advantages of simple principle and high detection precision.
Fig. 1 is a flow chart of a method for measuring the content of non-metal elements in lead bullion according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples, which are not intended to limit the scope of the invention.
1. About 200g of samples are taken from different positions of the crude lead, and the crude lead is cast into ingots in a lead mould. After cooling, turning a smooth plane by using a lathe, detecting all elements in a direct-reading spectrometer, and performing the same detection operation on the electrolytic lead;
2. cutting a sample of about 0.1g (accurate to 0.0001g) on a lead bullion by a knife, putting the sample into a beaker, digesting by nitric acid, and steaming until the sample is nearly dry; adding sulfuric acid, continuously steaming until a large amount of white smoke is emitted, stopping heating, and cooling; adding 30mL of distilled water along the wall of the cup, boiling and cooling. Then filtering with filter paper, washing the precipitate with distilled water, and transferring the filter paper and the precipitate into an original beaker; washing the wall of the cup with distilled water, adding 35mL of acetic acid-sodium acetate buffer solution, heating to boil, dropwise adding 1-2 drops of xylenol orange indicator, and titrating with a calibrated EDTA standard solution until the solution fades from red and then becomes bright yellow. And reading the consumption of the EDTA standard solution, and calculating the lead content of the lead bullion. The same detection operation is carried out on the electrolytic lead, and a sample with a smooth surface and no oxide film is required to be cut in the electrolytic lead sampling;
3. calculation of the filter coefficient: the spectrum detection result of the electrolytic lead is recorded as W1And the EDTA titration method has a detection result of w1The filtering coefficient is recorded as a, and the filtering coefficient is calculated according to the following formula:
a＝w1/W1；
4. in the EDTA titration process for determining lead content, a small amount of lead is lost during filtration. The filtration coefficient a represents the ratio of the lead content measured by EDTA to the real lead content under the same operation personnel and the same operation conditions;
5. calculating the real lead content in the crude lead:
the spectrum detection result of the crude lead is recorded as W2And the EDTA titration method has a detection result of w2Then its true lead content WPbI.e. w2The value corrected by the filter coefficient a, the real lead content WPbCalculated as follows:
WPb＝w2/a；
6. non-metal element W in crude leadOCalculated as follows:
WO＝W2－w2/a；
7. slag W of lead bullionSlagEstimation of (2): calculated according to the molar ratio of oxygen to sulfur in the crude lead dry slag of 1:1, the mixed molar mass is 24, WSlagCalculated as follows:
Wslag＝WO/24×231.2＝9.63WO；
The determination of non-metal elements and the estimation of slag rate are carried out on crude lead produced by a certain secondary lead factory, and the following steps are carried out:
the content of the obtained lead bullion nonmetal elements is 0.5518%, and the estimated lead slag content is 5.32%. The actual slag rate measured in the production process is about 5-6 percent and basically accords with the estimated result.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. A method for measuring non-metal elements in crude lead is characterized by comprising the following steps: the method comprises the following steps:
a. preparing an electrolytic lead sample, detecting by a direct-reading spectrometer, and recording the detection result as W1The electrolytic lead sample is detected by an EDTA titration method, and the detection result is recorded as w1；
b. Preparing a crude lead and lead ingot sample, and recording a detection result as W by a direct-reading spectrometer2The crude lead ingot sample is detected by EDTA titration method, and the detection result is recorded as w2；
c. The filtration coefficient a of the electrolytic lead is calculated according to the following formula:
a＝w1/W1；
d. correcting the lead bullion content w detected by EDTA titration by using the filtering coefficient a in the step c2Thereby obtaining the real lead content W of the crude leadPb(ii) a And then the content W of the lead bullion detected by a direct-reading spectrometer2Minus the true lead content WPbObtaining the content W of the non-metallic elementsOAnd characterizing the lead containing slag W of the lead bullion accordinglySlag。
2. The method for measuring the non-metallic elements in the lead bullion according to claim 1, characterized in that: the true lead content WPbThe value is the crude lead content w of EDTA determination after the filtration coefficient a correction2I.e. WPb＝w2/a。
3. The method of claim 2 for measuring non-metallic elements in bullionThe method is characterized in that: the content W of the non-metallic elementOOf value WO＝W2－w2/a。
4. The method for measuring the non-metallic elements in the lead bullion according to claim 3, characterized in that: the lead bullion containing slag WSlagOf value WSlagEstimated to be 9.63WO。
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Cited By (1)
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