CN110007046A - A method of measurement free lead content - Google Patents
A method of measurement free lead content Download PDFInfo
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- CN110007046A CN110007046A CN201910207518.5A CN201910207518A CN110007046A CN 110007046 A CN110007046 A CN 110007046A CN 201910207518 A CN201910207518 A CN 201910207518A CN 110007046 A CN110007046 A CN 110007046A
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- solution
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- sodium acetate
- free lead
- acetic acid
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005259 measurement Methods 0.000 title description 2
- 239000000243 solution Substances 0.000 claims abstract description 31
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 5
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 5
- 239000006210 lotion Substances 0.000 claims abstract description 5
- 208000030208 low-grade fever Diseases 0.000 claims abstract description 5
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 239000001632 sodium acetate Substances 0.000 claims abstract description 5
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 5
- 239000012086 standard solution Substances 0.000 claims abstract description 5
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 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 claims abstract description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 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 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 15
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000010998 test method Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000005070 sampling Methods 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000011505 plaster Substances 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 244000061458 Solanum melongena Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 1
- 239000004484 Briquette Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the present invention provides a kind of method for measuring free lead content, include the following steps, step 1, sample m grams, as Acetic acid-sodium acetate solution in 100mL beaker, is added, low-grade fever dissolves lead oxide；Step 2, upper solution is sucked out 2/3 with suction pipe, Acetic acid-sodium acetate washing lotion is added, a moment is stood after shaking up；Step 3, step 2 operation is repeated up to no precipitating；Step 4, add a little nitric acid solution and pure water, heat slightly boiled, dissolution free lead, and cooling；Step 5, add sodium acetate solution, ammonium hydroxide is added dropwise and is adjusted to solution ph；Step 6, add hexamethylenetetramine solution and xylenol orange, shake up；Step 7, it is titrated with EDETATE SODIUM standard solution；As a result it calculates:
Description
Technical field
The present invention relates to a kind of methods for measuring free lead content.
Background technique
The history of existing more than 150 years of invention of lead-acid accumulator, due to its good reliability, cost performance height, recoverable etc.
Advantage and be used widely.Requirement due to country to environmental protection in recent years, lead-acid accumulator are switched by tank formation technique
At internal formation process, pole plates used is all not pass through the green plate being melted into, after coated plate after solidifying and dividing brush program directly
Carry out battery assembly.The quality of green plate determines the performance of final battery after solidification, and one of cured main function is exactly lead
Free lead in cream aoxidizes, and optimizes curing process by the variation of solidification different phase sampling and testing free lead, by solid
Changing terminates green plate free lead, moisture and fall strength of briquette to determine cured effect.
Optimization curing process can be not only instructed by detection free lead numerical value change, is alternatively arranged as judging solidification effect
One of critical index, therefore be highly important to the detection of free lead.The method of standard testing free lead is at present: with taking
Sample cone quadrangle and intermediate bundle on pole plate take the sample of at least five single lattice, be put into it is finely ground in mortar after, weigh about 1g sample (essence
Really 40mL Acetic acid-sodium acetate solution is added, low-grade fever 15min keeps lead oxide completely molten as in 250mL conical flask to 0.0001g)
Solution, is filtered with fast grade filter paper, (checks filtrate with 20% sulfuric acid) until Acetic acid-sodium acetate washing lotion is washed till no lead ion, will
Filter paper and filter residue are moved into together in original 250mL conical flask, add 20mL (1:4) nitric acid solution and 20mL pure water, are heated slightly boiled
15min dissolves free lead, and slightly boiled removing nitrogen oxide, cold filtration is in 250mL conical flask.With pure water to unleaded
Ion (checks filtrate with 20% sulfuric acid), adds 5mL sodium acetate solution, ammonium hydroxide (1:1) is added dropwise to pH value of solution=5, adds 10mL six
Four amine aqueous solution of methine, 1~2 drop xylenol orange, solution should be in aubergine at this time, shake up.It is titrated with EDETATE SODIUM standard solution
Becoming glassy yellow to aubergine is terminal.
As a result it calculates:
In formula: C-EDTA molar concentration, unit are mole every liter (mol/L)
The volume of EDTA is consumed when V- is titrated, unit is milliliter (mL)
M- sample quality, unit of gram (g)
Need to extract entire curing room different location green plate detection free lead and moisture when detecting curing room homogeneity, it is excellent
It is needed when changing curing process in different curing time section sample detection pole plate free leads and moisture, the oxidation of lead plaster and containing for lead plaster
Water is to be mutually related, and water is the catalyst of lead oxidation reaction, and the heat that lead oxidation reaction is discharged causes in lead plaster
Water evaporation.Currently, the existing very quick and accurate detection method of moisture, and the detection method accurate detection method of free lead
Only described in top, a sample of detection is operated by this and takes around 2h, operation needs to filter twice, will increase error, secondary
When dissolution, it could be dissolved completely due to the presence of filter paper, needing to consume a large amount of nitric acid solution.It therefore, daily can only in production
By the way of sampling observation or test quantity is reduced to examine the quality of green plate, will cause some problematic curing rooms in this way
Missing inspection, problematic pole plate batch flow into next process, and final production goes out the underproof battery of performance；Adjust curing process
When, sampling observation pole plate cannot be measured in time as a result, lagging test free lead numerical value and actual value has deviation.Therefore, it quick and precisely surveys
It is very necessary, and above-mentioned in order to solve for determining free lead for guidance optimization curing process and the quality for determining green plate
Problem, it is necessary first to which a kind of method for finding out rapid and accurate determination free lead, CN105865966A disclose a kind of lead acid storage battery
The quick method for measuring of free lead in the green plate of pond, but its test process is very complicated, it is complicated for operation, it is also necessary to which that high-temperature vacuum dries
Dry-cure, test result data miss by a mile, and can not accurately react the content of free lead in green plate, in existing solidification process
Lack a kind of method of rapid and accurate determination pole plate free lead content.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of methods for measuring free lead content, including following step
Suddenly, step 1, m grams is sampled, as Acetic acid-sodium acetate solution in 100mL beaker, is added, low-grade fever dissolves lead oxide；Step 2, it uses
Upper solution is sucked out 2/3 by suction pipe, and Acetic acid-sodium acetate washing lotion is added, and a moment is stood after shaking up；Step 3, step 2 operation is repeated
Up to no precipitating；Step 4, add a little nitric acid solution and pure water, heat slightly boiled, dissolution free lead, and cooling；Step 5, add
Sodium acetate solution is added dropwise ammonium hydroxide and is adjusted to solution ph；Step 6, add hexamethylenetetramine solution and xylenol orange, shake up；Step
7, it is titrated with EDETATE SODIUM standard solution；
As a result it calculates:
In formula: C-EDTA molar concentration, unit are mole every liter (mol/L)
The volume of EDTA is consumed when V- is titrated, unit is milliliter (mL).
Test method of the invention, the testing time is few, easy to operate, saves chemical reagent, and test result is very accurate.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
The detection method of rapid and accurate determination free lead content of the present invention, specific operating procedure are as follows: step 1, sampling m
Gram, as Acetic acid-sodium acetate solution in 100mL beaker, is added, low-grade fever dissolves lead oxide；Step 2, with suction pipe upper solution
It is sucked out 2/3, Acetic acid-sodium acetate washing lotion is added, a moment is stood after shaking up；Step 3, step 2 is repeated to operate up to no precipitating,
Check suction pipe sucking liquid without precipitating with sulfuric acid；Step 4, add a little nitric acid solution and pure water, heat slightly boiled, dissolution trip
From lead, and cool down；Step 5, add sodium acetate solution, ammonium hydroxide is added dropwise and is adjusted to solution ph；Step 6, add hexamethylenetetramine solution
And xylenol orange, it shakes up；Step 7, it is titrated with EDETATE SODIUM standard solution；
As a result it calculates:
In formula: C-EDTA molar concentration, unit are mole every liter (mol/L)
The volume of EDTA is consumed when V- is titrated, unit is milliliter (mL)
M- sample quality, unit of gram (g)
A kind of detection method of rapid and accurate determination free lead content of the invention, is applicable not only to free lead in pole plate
Test, can also test the test of free lead in the substances such as lead powder and lead plaster, and this method not only can reduce the testing time, operation
Simplicity saves chemical reagent, and test result is also very accurate.Use the method can be to examine on Instructing manufacture in production
Degree of oxidation of lead powder；Determine that mixing paste to solidification terminates free lead changing rule；The quantity of sampling quantity for increasing pole plate after solidifying, to the greatest extent may be used
The unqualified green plate of evading of energy flows into next process.
Claims (1)
1. a kind of method for measuring free lead content, includes the following steps, step 1, m grams is sampled, as in 100mL beaker, is added
Enter Acetic acid-sodium acetate solution, low-grade fever dissolves lead oxide；Step 2, upper solution is sucked out 2/3 with suction pipe, acetic acid-acetic acid is added
Sodium washing lotion stands a moment after shaking up；Step 3, step 2 operation is repeated up to no precipitating；Step 4, add a little nitric acid solution
And pure water, slightly boiled, dissolution free lead is heated, and cooling；Step 5, add sodium acetate solution, ammonium hydroxide is added dropwise and is adjusted to solution ph；Step
Rapid 6, add hexamethylenetetramine solution and xylenol orange, shakes up；Step 7, it is titrated with EDETATE SODIUM standard solution；
As a result it calculates:
In formula: C-EDTA molar concentration, unit are mole every liter (mol/L)
The volume of EDTA is consumed when V- is titrated, unit is milliliter (mL).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910207518.5A CN110007046A (en) | 2019-03-19 | 2019-03-19 | A method of measurement free lead content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910207518.5A CN110007046A (en) | 2019-03-19 | 2019-03-19 | A method of measurement free lead content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110007046A true CN110007046A (en) | 2019-07-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910207518.5A Pending CN110007046A (en) | 2019-03-19 | 2019-03-19 | A method of measurement free lead content |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113433024A (en) * | 2021-06-01 | 2021-09-24 | 风帆有限责任公司 | Method for detecting porosity of negative plate after formation of start-stop AGM battery |
| CN114544418A (en) * | 2022-01-27 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Polar plate performance determination method based on positive plate grid corrosion layer and paste adhesion of lead storage battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102426168A (en) * | 2011-09-22 | 2012-04-25 | 重庆万里控股（集团）股份有限公司 | Method for determining free lead in lead-acid storage battery green plate sample |
| CN105865966A (en) * | 2016-03-22 | 2016-08-17 | 超威电源有限公司 | Rapid determination method for free lead in green plate of lead acid battery |
-
2019
- 2019-03-19 CN CN201910207518.5A patent/CN110007046A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102426168A (en) * | 2011-09-22 | 2012-04-25 | 重庆万里控股（集团）股份有限公司 | Method for determining free lead in lead-acid storage battery green plate sample |
| CN105865966A (en) * | 2016-03-22 | 2016-08-17 | 超威电源有限公司 | Rapid determination method for free lead in green plate of lead acid battery |
Non-Patent Citations (1)
| Title |
|---|
| 中国国家标准化管理委员会等: "《中华人民共和国国家标准》", 12 May 2017 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113433024A (en) * | 2021-06-01 | 2021-09-24 | 风帆有限责任公司 | Method for detecting porosity of negative plate after formation of start-stop AGM battery |
| CN113433024B (en) * | 2021-06-01 | 2022-08-23 | 风帆有限责任公司 | Method for detecting porosity of negative plate after formation of start-stop AGM battery |
| CN114544418A (en) * | 2022-01-27 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Polar plate performance determination method based on positive plate grid corrosion layer and paste adhesion of lead storage battery |
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Address after: 313100 Zhejiang city of Huzhou province Changxing County pheasant emerging urban industrial park Applicant after: Chaowei Power Group Co., Ltd Address before: 313199 new industrial park, pheasant Town, Huzhou, Zhejiang, Changxing County Applicant before: Chilwee Power Supply Co., Ltd. |
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Application publication date: 20190712 |