CN106092925B - The assay method of gelatine effective content in borofluoride electro-deposition lead solution - Google Patents
The assay method of gelatine effective content in borofluoride electro-deposition lead solution Download PDFInfo
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- 239000001828 Gelatine Substances 0.000 title claims abstract description 64
- 229920000159 gelatin Polymers 0.000 title claims abstract description 64
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 64
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 58
- 238000003556 assay Methods 0.000 title claims abstract description 11
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 43
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 10
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 10
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 10
- 229940033123 tannic acid Drugs 0.000 claims abstract description 10
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 10
- 229920002258 tannic acid Polymers 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims abstract description 4
- 230000003472 neutralizing effect Effects 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 48
- 238000004364 calculation method Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 239000012085 test solution Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 48
- 239000002659 electrodeposit Substances 0.000 abstract description 39
- 238000001514 detection method Methods 0.000 abstract description 25
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000012423 maintenance Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 25
- 239000012488 sample solution Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 19
- 238000006386 neutralization reaction Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- 238000000151 deposition Methods 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 2
- 239000002639 bone cement Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 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 description 1
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- -1 nitric acid Ion Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
Abstract
The invention belongs to technical field of battery production, and in particular to the assay method of gelatine effective content in a kind of borofluoride electro-deposition lead solution.The lead ion in electro-deposition lead solution is removed, then neutralizing makes electro-deposition lead solution be in neutrality, and nitrate ion content is measured using ultraviolet-visible spectrophotometry；Pipette samples electro-deposition lead solution is placed in beaker, and tannic acid solution is added under constant stirring, is placed, and filtering is washed with water to neutrality, dries to constant weight in an oven, weighs the weight of precipitation, calculates the content of gelatine in sample electro-deposition lead solution.The content of nitrate anion impurity and the content of gelatine in energy Accurate Determining borofluoride electro-deposition lead solution of the invention, solve the problems, such as that gelatine content detection error is larger in borofluoride electro-deposition lead solution, it can be used for instructing the maintenance of borofluoride electro-deposition splicer's skill, improve the stability of electrodeposit liquid, production cost is saved, environmental pollution is reduced.
Description
Technical field
The invention belongs to technical field of battery production, and in particular to gelatine is effective in a kind of borofluoride electro-deposition lead solution
The assay method of content.
Background technology
A small amount of gelatine in borofluoride electro-deposition lead liquid is the crystallization of refinement lead deposit layer, prevents the plating leakage of lead deposit layer and production
Additive necessary to raw ingotism.In electrodeposition process, the organic macromolecule in gelatine is adsorbed in cathode surface, is increased
The overpotential of leading deposition, keeps crystallization careful, improves the dispersibility of deposition liquid.Commonly gelatine content detection principle is：It is logical
The flocculation for crossing tannic acid and bone glue protein, through filtering and drying, the weight is agglomerated in weighing, and electrodeposit liquid is calculated with this
The effective content of middle gelatine.
In actual production, electro-deposition pretreatment procedure, which is brought into the impurity of electrodeposit liquid, can influence the detection of gelatine content
With the quality of electro-deposition, wherein nitrate anion foreign ion present in electrodeposit liquid is for gelatine content detection and electro-deposition quality
Influence it is the most notable.
The nitrate ion brought into electrodeposition process is adsorbed in cathode surface, in cathode surface nitrate anion and bone
There are a large amount of nitre when the too high levels of nitrate ion in solution in cathode surface in organic macromolecule competitive Adsorption in glue
The position of acid ion absorption, the deposition of lead ion is hindered, causes to leak depositional phenomenon, influences product quality.Contain in gelatine
The addition of nitrate anion impurity, which destroys protein and the flocculation of tannic acid, in the detection process of amount, in deposition liquid causes to precipitate
The reduction of weight, test gained gelatine content reduce, and the addition of nitrate anion destroys the accurate measurement of gelatine, influences electrodeposit liquid
Maintenance use.
Therefore the effective content for how effectively measuring the nitrate anion foreign ion and gelatine in electrodeposit liquid, for improving electricity
The stability of deposition quality and electrodeposit liquid has a major impact.The country is less for the research of borofluoride deposit lead liquid, about
The researches of its additive gelatine and foreign ion nitrate anion, most of deposit lead manufacturer are passed through according to production
It tests, increases the content of additive and other components, carry out the maintenance of electrodeposit liquid, electrodeposit liquid is useless when depositing liquid and can not safeguard
It abandons, causes serious environmental pollution and economic waste.
Invention content
The object of the present invention is to provide a kind of assay method of gelatine effective content in borofluoride electro-deposition lead solution, sections
Learn reasonable, simple and practicable, the content of nitrate anion impurity and the content of gelatine in energy Accurate Determining borofluoride electro-deposition lead solution.
The assay method of gelatine effective content in borofluoride electro-deposition lead solution of the present invention, steps are as follows：
(1) remove electro-deposition lead solution in lead ion, then neutralize so that electro-deposition lead solution is in neutrality, using it is ultraviolet can
Light-exposed spectrophotometry measures nitrate ion content；
(2) pipette samples electro-deposition lead solution 20mL is placed in beaker, and the tannic acid that 50g/L is added under constant stirring is molten
Liquid 20mL is placed, and is filtered with the Gooch crucible for being covered with filter paper in advance and drying to constant weight, neutrality is washed with water to, in baking oven
In dry to constant weight, weigh the weight y of precipitation；
(3) gelatine calculation formula：
Gelatine=13.801 × y-0.135 is 1.
Gelatine=14.551 × y-0.185 is 2.
Gelatine=15.473 × y-0.234 is 3.
As nitrate ion concentration≤0.04mol/L, formula can be used and 1. calculate gelatine in sample electro-deposition lead solution
Content；As 0.04mol/L ＜ nitrate ion concentrations≤0.06mol/L, formula can be used and 2. calculate sample electro-deposition lead
The content of gelatine in solution；As 0.06mol/L ＜ nitrate ion concentrations≤0.08mol/L, formula can be used and 3. calculate sample
The content of gelatine in product electro-deposition lead solution.
Standing time described in step (2) is 15min.
Oven temperature described in step (2) is 105-110 DEG C.
The present invention excludes the influence that other ions measure nitrate ion in borofluoride electro-deposition lead solution, according to
The correspondence formula of nitrate radical content and gelatine effective content, can in Accurate Determining electrodeposit liquid gelatine effective content,
Within the scope of different nitrate radical contents, corresponding gelatine calculation formula is different.
The assay method of gelatine effective content in borofluoride electro-deposition lead solution of the present invention, specific steps are such as
Under：
Lead ion removal and neutralization method in 1 borofluoride electro-deposition lead solution
1.1 methods are made a summary
Lead ion and hydrogen ion in electrodeposit liquid seriously affect the testing result of nitrate ion, need to remove lead ion
And electrodeposit liquid is made to be in neutrality.
1.2 reagents and instrument
Litmus reagent, standard 0.1N sodium hydroxide solutions, 0.1N standard sulfuric acid solutions, 10N standard caustic soda solutions,
10N standard sulfuric acid solutions.
1.3 lead ions and hydrogen ion removal step
1) removal of lead ion
The borofluoride electro-deposition lead sample solution that 10mL is taken with pipette, is titrated with 0.1N standard sulfuric acid solutions,
Until solution no longer generates precipitation, record uses the volume L of 0.1N standard sulfuric acid solutions.
The electro-deposition lead sample solution for taking 1L is slowly added to the 10N standard sulfuric acid solutions of L while stirring, makes them fully
Reaction makes lead ion precipitate completely, and the electrodeposit liquid after removal lead ion is obtained with filter paper filtering precipitation, measures its volume V1.
2) neutralization of sample solution
Electrodeposit liquid after taking 10mL to remove lead ion with pipette drips 3-5 drop litmus reagents, with 0.1N standard hydroxides
Sodium solution is titrated, until solution from it is colourless just become red when stop, record is using 0.1N standard caustic soda solutions
Volume M.
It takes 1L except the electrodeposit liquid after lead, is slowly added to the 10N standard caustic soda solutions of M while stirring, them is made to fill
Divide reaction, measures the volume V2 of sample solution after reaction.
The measurement of 2 nitrate ion contents
Nitrate ion is measured using ultraviolet-visible spectrophotometry.
2.1 methods are made a summary
UV-VIS spectrophotometry can be used in the measurement of nitrate anion, is typically chosen in measurement nitrate ion at 220nm
Concentration.Reference《The survey ultraviolet spectrophotometry (tentative) (HJ_T 346-2007) of water quality nitrate nitrogen》It carries out.
2.2 reagents and instrument
Tu-1901 dual-beams ultraviolet-uisible spectrophotometer (900-190nm), the ultraviolet software v5.0.5 of UVWin5, capacity
Bottle, cuvette, pipette.
The detecting step of 2.3 nitrate ion contents
1) preparation of nitrate anion titer
To remove the electrodeposit liquid without containing nitrate ion after lead ion and neutralisation treatment as solvent, prepares and contain nitric acid
Ion concentration is that the standard electro-deposition of 0.02mol/L, 0.04mol/L, 0.06mol/L, 0.08mol/L, 0.10mol/L are molten
Liquid tests its curve of spectrum under various concentration.Maximum absorption band of the nitrate ion in the solution at 202.5nm,
According to Beer law, the corresponding formula of absorbency Y at 202.5nm (Abs) and nitrate ion concentration X (mol/L) is obtained
For Y=9.345*X-0.0017 (similarity R=0.9998).
2) in sample electrodeposit liquid nitrate ion content detection
It removes except the electrodeposit liquid sample after lead ion and neutralisation treatment, is existed with optical length 10mm quartz colorimetric utensils
The measurement of absorbance is carried out at 202.5nm.It is more than such as range, N times can be diluted to electrodeposit liquid sample, then determination sample
The absorbency Y of electrodeposit liquid.
2.4 calculating
The content calculation formula of nitrate ion in sample electrodeposit liquid：
X=(Y+0.0017) × N × V1 × V2/9.345 2-1
In formula：The content (mol/L) of X --- the nitrate ion in sample electrodeposit liquid；
Absorbance value (Abs) of Y --- the sample electrodeposit liquid at 202.5nm absorption peaks；
N --- electrodeposit liquid sample extension rate；
Volume (L) after the sample electric depositing solution removal lead ion of V1 --- 1L；
Volume (L) after the removal lead ion of V2 --- 1L after electric depositing solution neutralisation treatment.
The assay method of 3 gelatine
3.1 methods are made a summary
Bone glue protein is acted on tannic acid and is agglomerated in sample, and through filtering drying, the weight and calculating are agglomerated in weighing
The content of gelatine.
3.2 reagents and instrument
Tannic acid, Gooch crucible, baking oven, beaker, filter paper.
3.3 determination step
Pipette samples electrodeposit liquid 20mL is placed in 100mL beakers, and tannic acid solution 20mL is added under constant stirring, puts
15min is set, is filtered with the Gooch crucible for being covered with filter paper in advance and drying to constant weight, neutrality is washed with water to, at 105-110 DEG C
Baking oven in dry to constant weight, weigh the weight y of precipitation.
3.4 calculating
Gelatine calculation formula：
Gelatine (g/L)=13.801 × y-0.135 is 1.
Gelatine (g/L)=14.551 × y-0.185 is 2.
Gelatine (g/L)=15.473 × y-0.234 is 3.
The weight (g) of y- precipitations；
(1) as nitrate ion concentration≤0.04mol/L, formula can be used and 1. calculate bone in sample electro-deposition lead solution
The content of glue；As 0.04mol/L ＜ nitrate ion concentrations≤0.06mol/L, formula can be used and 2. calculate sample electro-deposition
The content of gelatine in lead solution；As 0.06mol/L ＜ nitrate ion concentrations≤0.08mol/L, formula can be used and 3. calculate
The content of gelatine in sample electro-deposition lead solution.
(2) calculation formula is only applicable in 20mL test solutions this condition of the tannic acid 20mL of 50g/L that adds, if change this condition
The formula cannot be used.
(3) precipitation capacity is thinner when the temperature is low, easily penetrates filter paper layer, therefore when temperature is less than 10 DEG C, slightly hot it should be kept solidifying
It is poly-.
Compared with prior art, the present invention having the advantages that：
The content of nitrate anion impurity and the content of gelatine in energy Accurate Determining borofluoride electro-deposition lead solution of the invention, solution
The larger problem of gelatine content detection error in borofluoride electro-deposition lead solution of having determined, can be used for instructing borofluoride electro-deposition
The maintenance of splicer's skill improves the stability of electrodeposit liquid, saves production cost, reduces environmental pollution.
Specific implementation mode
The present invention is described further with reference to embodiments.
Embodiment 1
With copper coin grid electro-deposition lead workshop 1# station sample solution explanations
Copper coin grid electro-deposition lead workshop 1# station sample solutions are taken, lead is removed according to 1.3 in present invention prescriptive procedures
Ion and neutralisation treatment, while it is 1.10L, the electro-deposition after neutralisation treatment to measure the electrodeposit liquid volume V1 after removal lead ion
It is 1.24L that liquid, which accumulates V2,.It removes except the electrodeposit liquid sample after lead ion and neutralisation treatment, according to 2.3 in present invention rule
Determine the measurement that method carries out absorbance with optical length 10mm quartz colorimetric utensils at 202.5nm, the absorbency Y of sample electrodeposit liquid
It is 0.019, the content X that the nitrate ion in sample electrodeposit liquid is calculated according to formula 2-1 is 0.003mol/L.Take copper
Grid electro-deposition lead workshop 1# station sample solution 20mL, the y values of sample solution are obtained according to 3.3 in present invention prescriptive procedures
For 0.089g.
The specific test data of the sample solution is shown in Table 1.
1 sample solution testing result of table
| Detection project | V1(L) | V2(L) | N | Y(Abs) | X(mol/L) | Y(g) |
| Detection data | 1.10 | 1.24 | 1 | 0.019 | 0.003 | 0.089 |
According to the testing result of table 1, the content of nitrate ion is 0.003mol/L, the use condition of coincidence formula 1.,
The inspection result comparison of gelatine content is shown in Table 2.
2 gelatine content detection Comparative result of table
| Project | Former detection method | Detection method | Actual numerical value |
| Gelatine content (g/L) | 0.935 | 1.093 | 1.20 |
Using detection method acquired results closer to actual numerical value.
Embodiment 2
With copper coin grid electro-deposition lead workshop 9# station sample solution explanations
Copper coin grid electro-deposition lead workshop 9# station sample solutions are taken, lead is removed according to 1.3 in present invention prescriptive procedures
Ion and neutralisation treatment, while it is 1.15L, the electro-deposition after neutralisation treatment to measure the electrodeposit liquid volume V1 after removal lead ion
It is 1.22L that liquid, which accumulates V2,.It removes except the electrodeposit liquid sample after lead ion and neutralisation treatment, according to 2.3 in present invention rule
Determine the measurement that method carries out absorbance with optical length 10mm quartz colorimetric utensils at 202.5nm, the absorbency Y of sample electrodeposit liquid
It is 0.005, the content X that the nitrate ion in sample electrodeposit liquid is calculated according to formula 2-1 is 0.001mol/L.Take copper
Grid electro-deposition lead workshop 9# station sample solution 20mL, the y values of sample solution are obtained according to 3.3 in present invention prescriptive procedures
For 0.147g.
The specific test data of the sample solution is shown in Table 3.
3 sample solution testing result of table
| Detection project | V1(L) | V2(L) | N | Y(Abs) | X(mol/L) | Y(g) |
| Detection data | 1.15 | 1.22 | 1 | 0.005 | 0.001 | 0.147 |
According to the testing result of table 3, the content of nitrate ion is 0.001mol/L, the use condition of coincidence formula 1.,
The inspection result comparison of gelatine content is shown in Table 4.
4 gelatine content detection Comparative result of table
| Project | Former detection method | Detection method | Actual numerical value |
| Gelatine content (g/L) | 1.648 | 1.894 | 2.00 |
Using detection method acquired results closer to actual numerical value.
Embodiment 3
With copper coin grid electro-deposition lead workshop waste sample solution explanation
Take copper coin grid electro-deposition lead workshop waste sample solution, according in the present invention 1.3 prescriptive procedures removal lead from
Son and neutralisation treatment, while it is 1.17L, the electrodeposit liquid after neutralisation treatment to measure the electrodeposit liquid volume V1 after removal lead ion
Volume V2 is 1.27L.It removes except the electrodeposit liquid sample after lead ion and neutralisation treatment, according to 2.3 in present invention regulations
Method carries out the measurement of absorbance with optical length 10mm quartz colorimetric utensils at 202.5nm, and the absorbency Y of sample electrodeposit liquid is
0.156, the content X that the nitrate ion in sample electrodeposit liquid is calculated according to formula 2-1 is 0.025mol/L.Take copper coin
Grid electro-deposition lead workshop waste sample solution 20mL, the y values that sample solution is obtained according to 3.3 in present invention prescriptive procedures are
0.244g。
The specific test data of the sample solution is shown in Table 5.
5 sample solution testing result of table
| Detection project | V1 | V2 | N | Y | X | y |
| Detection data | 1.17 | 1.27 | 1 | 0.156 | 0.025 | 0.244 |
According to the testing result of table 5, the content of nitrate ion is 0.025mol/L, the use condition of coincidence formula 1.,
The inspection result comparison of gelatine content is shown in Table 6.
6 gelatine content detection Comparative result of table
| Project | Former detection method | Detection method |
| Gelatine content (g/L) | 2.841 | 3.232 |
The technique content of gelatine is between (1.0-3.0) g/L in copper coin grid electro-deposition lead solution, using detection side of the invention
The content of gelatine is more accurate in waste sample solution obtained by method.
Claims (3)
1. the assay method of gelatine effective content in a kind of borofluoride electro-deposition lead solution, it is characterised in that steps are as follows：
（1）The lead ion in electro-deposition lead solution is removed, then neutralizing makes electro-deposition lead solution be in neutrality, using ultraviolet-visible
Spectrophotometry measures nitrate ion content；
（2）Pipette samples electro-deposition lead solution 20mL is placed in beaker, and the tannic acid solution of 50g/L is added under constant stirring
20mL is placed, and is filtered with the Gooch crucible for being covered with filter paper in advance and drying to constant weight, is washed with water to neutrality, in an oven
It dries to constant weight, the unit for weighing the weight y, y of precipitation is g；
（3）Gelatine content calculation formula：
Gelatine content=13.801 × y -0.135 is 1.
Gelatine content=14.551 × y -0.185 is 2.
Gelatine content=15.473 × y -0.234 is 3.
Calculation formula is only applicable in 20mL test solutions this condition of the tannic acid 20mL of 50g/L that adds, if cannot make when changing this condition
With the formula；
As nitrate ion concentration≤0.04mol/L, formula can be used and 1. calculate containing for gelatine in sample electro-deposition lead solution
Amount；As 0.04mol/L ＜ nitrate ion concentrations≤0.06mol/L, formula can be used and 2. calculate sample electro-deposition lead solution
The content of middle gelatine；As 0.06mol/L ＜ nitrate ion concentrations≤0.08mol/L, formula can be used and 3. calculate sample electricity
Deposit the content of gelatine in lead solution；The unit of gelatine content is g/L.
2. the assay method of gelatine effective content, feature in borofluoride electro-deposition lead solution according to claim 1
It is step（2）Described in standing time be 15min.
3. the assay method of gelatine effective content, feature in borofluoride electro-deposition lead solution according to claim 1
It is step（2）Described in oven temperature be 105-110 DEG C.
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