CN105891201A - Method for detecting content of formaldehyde in alkaline electroless copper plating waste water - Google Patents
Method for detecting content of formaldehyde in alkaline electroless copper plating waste water Download PDFInfo
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- CN105891201A CN105891201A CN201610208303.1A CN201610208303A CN105891201A CN 105891201 A CN105891201 A CN 105891201A CN 201610208303 A CN201610208303 A CN 201610208303A CN 105891201 A CN105891201 A CN 105891201A
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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
- G01N21/75—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
Abstract
The invention provides a method for detecting the content of formaldehyde in alkaline electroless copper plating waste water. The method comprises the steps that Cu<2+> in a solution is removed with sodium sulfide, strong acid is added to remove excess hydrogen sulfide, a 20% sodium hydroxide solution and an iodine standard solution are added, standing reacting is conducted, and under the acidic condition, quantitative titration is conducted with sodium thiosulfate. According to the method for detecting the content of formaldehyde in the alkaline electroless copper plating waste water, detection is not disturbed by other positive ions and negative ions in an aqueous solution, and the content of formaldehyde can be determined easily and accurately.
Description
Technical field
The present invention relates to the technical field of analysis and detection of a kind of content of formaldehyde, especially relate to the alkalization of a kind of mensuration
Learn the method for content of formaldehyde in copper plating bath.
Background technology
Formaldehyde is the colourless flammable liquid with pungent odour, soluble in water, alcohol and ether, and it is 35%～40% years old
The aqueous solution be referred to as " formalin ", belong to relatively high toxic material, at home toxic chemical priority acccess control
Second it is on list.The reproducibility of formaldehyde is very strong, is easily combined with many kinds of substance, and is prone to polymerization.Right
Human central nervous system, retina, lung and liver have and damage more by force, can trigger endocrine dysfunction and
Skin disease, is defined as carcinogenic and teratogen by the World Health Organization." water environment quality standard " and
Concentration of formaldehyde in water has all been done strict restriction by " Drinking Water hygienic quality specification ".The main dirt of formaldehyde
Dye derives from the useless of the industry discharges such as organic synthesis, chemical industry, synthetic fibers, dyestuff, timber processing and painting
Water.After waste water containing formaldehyde enters water body, the dissolved oxygen in water can be consumed, affect the self-purification capacity of water.By
This apparently, the quantitatively detection of formaldehyde is critically important in aqueous.
Analyzing detecting method about content of formaldehyde mainly has titration, colorimetric method, oscilloscopic polarography and height at present
Effect liquid phase chromatogram method etc..But wherein oscilloscopic polarography and high performance liquid chromatography need to carry out sample strictly
Pre-treatment, in oscilloscopic polarography use dropping-mercury electrode there is pollution hidden trouble, high performance liquid chromatography instrument hold high
Expensive, the requirement to operating personnel is higher.Titration uses starch to be the titration of indicator sodium thiosulfate, because changing
Learn in copper plating solution and there is copper ion, affect measurement result.Colorimetric method is because chemical copper plating solution itself is existing
Color, affects Colorimetric results.Above-mentioned several method is unsuitable for measuring content of formaldehyde in chemical bronze plating liquid.Cause
This, be badly in need of a kind of measuring the method for content of formaldehyde in chemical copper plating solution.
Summary of the invention
The problems referred to above existed for prior art, the applicant provides a kind of detection alkaline chemical copper plating waste liquid
The method of middle content of formaldehyde.This method detection is not disturbed by other cation and anion in the aqueous solution, can
To measure the content of formaldehyde simply, accurately.
Technical scheme is as follows:
A kind of detect the method for content of formaldehyde in alkaline chemical copper plating waste liquid, including following detecting step:
(1) the copper content in Accurate Determining alkaline chemical copper plating waste liquid；
(2) adjust pH ＞ 10, add vulcanized sodium so that copper content is 1:1-5 with the mol ratio of vulcanized sodium, stirring
Make it react, stand and filter；
(3) taking above-mentioned filtrate 50mL, the HCl being slowly added to 5-30wt% regulates pH ＜ 1, and stirring is to nothing
Hydrogen sulfide gas produce, after be settled to 100mL；
(4) take above-mentioned solution 5.00ml, add 10ml 20wt% sodium hydroxide solution；
(5) accurately adding 10.00ml 0.1mol/L iodine standard solution, fluid-tight shakes up, and stands 5-60 in dark place
min；
(6) 10ml 10-30wt% sulfuric acid solution is added；
(7) it is titrated to faint yellow with 0.1mol/L sodium thiosulfate standard solution, adds 2ml 0.5wt% starch
Indicator, continues to drop to blueness and just disappears, and record consumes the volume of sodium thiosulfate standard solution；
(8) it is calculated as follows content of formaldehyde:
Wherein, CI2For iodine mark liquid concentration, mol/L, VI2Amass for iodine mark liquid, ml；CNa2S2O4For sulphur for sulphur
Acid na concn, mol/L；VNa2S2O4For sodium thiosulfate volume, ml；MHCHOFor formaldehyde molal weight,
g/mol；VSample: pipette and treat test sample volume, ml；CHCHOFor content of formaldehyde, g/L.
After removing copper with vulcanized sodium, titration results is not by the shadow of other cations in Chemical Copper Plating Effluent
Ring.After removing unnecessary vulcanized sodium after adding HCl acid by step (3), titration results is not by other anion
The impact of (sulphion).
Useful the having the technical effect that of the present invention
Patent of the present invention is given up mainly for the mensuration of content of formaldehyde in alkaline chemical copper plating waste liquid, alkaline chemical copper plating
The assay method that in liquid, copper content content of formaldehyde in 0.5-2g/L, chemical bronze plating liquid is traditional is iodimetric titration, this method
In the presence of planar defect:
1, during measuring, copper ion and iodide ion are easily formed cuprous iodide and cause Lower result；
2, there is ammonium salt in Chemical Copper Plating Effluent, react with formaldehyde and generate six formaldehyde tetramines:
6HCHO+4NH4 +=(CH2)6N4H++3H++6H2O
This reaction is reversible reaction, also can have an impact for the result finally recorded.
Comparatively speaking, present invention have the advantage that
1, detection architecture low cost；
2, detection is quantitative, and its content after vulcanized sodium removes of the metal ion in solution can be less than 0.5mg/L,
On testing result without impact；
3, titration system is acid, and ammonium radical ion therein is on detection nothing impact；
4, detection environment is to carry out in aqueous；
Therefore, this invention is also applied to the detection of content of formaldehyde in environmental water systems or chemical plating.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is specifically described.Embodiment refers to Chemical Copper Plating Effluent, but
It is that this method can measure content of formaldehyde in the solution of any cupric and formaldehyde.
Embodiment 1:
Taking 100mL alkaline chemical copper plating waste liquid, copper content is 250mg/L, adjusts pH ＞ 10, presses
nCu2+:Na2The amount of S=1:0.5 (ratio that n represents below is mol ratio) adds 0.0154g vulcanized sodium solid,
Stirring reaction 20min, filters；Accurately pipette filtrate 50.00mL in clean 100mL glass beaker, slow
The slow 20%HCl of addition regulates pH ＜ 1, stirring 15min and guarantees that sulphion volatilizees with hydrogen sulfide form completely,
Transfer is settled to 100mL.Accurately pipette above-mentioned solution 5.00mL, add 10ml 20% sodium hydroxide solution,
Shake up；Accurately adding 10.00ml 0.1556mol/L iodine standard solution, fluid-tight shakes up, and stands 10min in dark place；
It is eventually adding 10ml 20% sulfuric acid solution, is titrated to 0.1255mol/L sodium thiosulfate standard solution rapidly
Faint yellow, add 2ml 0.5% starch indicator, continue to drop to blueness and just disappear, record consumes sulphur for sulphur
Acid sodium standard solution 23.98mL, calculating concentration of formaldehyde in alkali electroless copper solution according to formula is
0.308g/L。
Embodiment 2:
Taking 100mL alkaline chemical copper plating waste liquid, copper content is 250mg/L, adjusts pH ＞ 10, presses
nCu2+:Na2The amount of S=1:1 adds 0.0308g vulcanized sodium solid, stirring reaction 20min, filters；Accurately move
Take filtrate 50.00mL in clean 100mL glass beaker, be slowly added to 20%HCl and regulate pH ＜ 1, stir
Mixing 15min and guarantee that sulphion volatilizees with hydrogen sulfide form completely, transfer is settled to 100mL.Accurately pipette
State solution 5.00mL, add 10ml 20% sodium hydroxide solution, shake up；Accurately add 10.00ml 0.1556
Mol/L iodine standard solution, fluid-tight shakes up, and stands 10min in dark place；It is eventually adding 10ml 20% sulfuric acid molten
Liquid, is titrated to faint yellow with 0.1255mol/L sodium thiosulfate standard solution rapidly, adds 2ml 0.5% and forms sediment
Powder indicator, continues to drop to blueness and just disappears, and record consumes sodium thiosulfate standard solution
23.61mL/23.64mL, calculating concentration of formaldehyde according to formula is 0.447g/L.
Embodiment 3:
Blank assay: take 2.00mL and analyze pure formalin, be settled to 100mL, accurately pipette 5.00mL,
Add 10ml 20% sodium hydroxide solution, shake up；Accurately add 10.00ml 0.1556mol/L iodine standard molten
Liquid, fluid-tight shakes up, and stands 10min in dark place；It is eventually adding 10ml 20%HCl solution, rapidly with 0.1255
Mol/L sodium thiosulfate standard solution is titrated to faint yellow, adds 2ml 0.5% starch indicator, continues to drip
Just disappearing to blueness, record consumes sodium thiosulfate standard solution volume 1.82mL, calculates according to formula
Concentration of formaldehyde is 432.971g/L.
Embodiment 4:
Taking 100mL alkali electroless copper solution, copper content is 250mg/L, adjusts pH ＞ 10, by nCu2+:Na2S=1:3
Amount add 0.0308g vulcanized sodium solid, stirring reaction 20min, filter；Accurately pipette filtrate 50.00mL
In clean 100mL glass beaker, it is slowly added to 20%HCl and regulates pH ＜ 1, stir 15min and guarantee sulphur
Ion volatilizees with hydrogen sulfide form completely, and transfer is settled to 100mL.Accurately pipette above-mentioned solution 5.00mL,
The most accurately add 0.1mL and analyze pure formaldehyde, add 10ml 20% sodium hydroxide solution, shake up；Accurately add
10.00ml 0.1556mol/L iodine standard solution, fluid-tight shakes up, and stands 10min in dark place；It is eventually adding 10
Ml 20%HCl solution, is titrated to faint yellow with 0.1255mol/L sodium thiosulfate standard solution rapidly, adds
2ml 0.5% starch indicator, continues to drop to blueness and just disappears, and record consumes sodium thiosulfate standard solution
Volume 1.12mL, calculating concentration of formaldehyde according to formula is 8.923g/L.
Embodiment 5:
Accurately weigh 0.025g and analyze pure copper chloride, accurately add the 2.00mL pure formaldehyde of analysis and be dissolved in 50mL water,
Then 100mL it is settled to；Above-mentioned solution is adjusted pH ＞ 10, in molar ratio nCu2+:Na2The amount of S=1:1 adds
Vulcanized sodium solid, stirring reaction 20min, filters；Accurately pipette filtrate 50.00mL in clean 100mL glass
In glass beaker, it is slowly added to 20%HCl and regulates pH ＜ 1, stir 15min and guarantee that sulphion is completely with sulfuration
Hydrogen form volatilizees, and transfer is settled to 100mL.Accurately pipette above-mentioned solution 5.00mL, add 10ml 20%
Sodium hydroxide solution, shakes up；Accurately adding 10.00ml 0.1556mol/L iodine standard solution, fluid-tight shakes up,
10min is stood in dark place；It is eventually adding 10ml 20% sulfuric acid solution, rapidly with 0.1255mol/L sulphur for sulphur
Acid sodium standard solution is titrated to faint yellow, adds 2ml 0.5% starch indicator, continues to drop to blueness and just disappear
Losing, record consumes sodium thiosulfate standard solution volume 1.83mL, and in the most above-mentioned self-made solution, content of formaldehyde is
8.66g/L.It is 866mg that detection obtains adding formaldehyde amount, and actual additional formaldehyde amount is 865.9mg.
Embodiment 6:
Accurately weigh 0.025g and analyze pure copper chloride, be dissolved in 50mL water, be then settled to 100mL；By above-mentioned
Solution adjusts pH ＞ 10, in molar ratio nCu2+:Na2The amount of S=1:1 adds vulcanized sodium solid, and 20min is reacted in stirring,
Filter；Accurately pipette filtrate 50.00mL in clean 100mL glass beaker, be slowly added to 20%HCl
Regulation pH ＜ 1, stirring 15min guarantee that sulphion vapors away with hydrogen sulfide form completely, then shift constant volume
To 100mL.Accurately pipette above-mentioned solution 5.00mL, add 10ml 20% sodium hydroxide solution, shake up；
Accurately adding 10.00ml 0.1556mol/L iodine standard solution, fluid-tight shakes up, and stands 10min in dark place；?
Rear addition 10ml 20% sulfuric acid solution, is titrated to light with 0.1255mol/L sodium thiosulfate standard solution rapidly
Yellow, adds 2ml 0.5% starch indicator, continues to drop to blueness and just disappear, and record consumes thiosulfuric acid
Sodium standard solution volume 24.80mL, calculating concentration of formaldehyde is 0g/L.
Embodiment 7:
Accurately weigh 0.025g and analyze pure copper chloride, accurately add the 2.00mL pure formaldehyde of analysis and be dissolved in 50mL water,
Then 100mL it is settled to；Above-mentioned solution is adjusted pH ＞ 10, in molar ratio nCu2+:Na2The amount of S=1:5 adds
Vulcanized sodium solid, stirring reaction 20min, filters；Accurately pipette filtrate 50.00mL in clean 100mL glass
In glass beaker, it is slowly added to 20%HCl and regulates pH ＜ 1, stir 15min and guarantee that sulphion is completely with sulfuration
Hydrogen form volatilizees, and transfer is settled to 100mL.Accurately pipette above-mentioned solution 5.00mL, add 10ml 20%
Sodium hydroxide solution, shakes up；Accurately adding 10.00ml 0.1556mol/L iodine standard solution, fluid-tight shakes up,
10min is stood in dark place；It is eventually adding 10ml 20% sulfuric acid solution, rapidly with 0.1255mol/L sulphur for sulphur
Acid sodium standard solution is titrated to faint yellow, adds 2ml 0.5% starch indicator, continues to drop to blueness and just disappear
Losing, record consumes sodium thiosulfate standard solution volume 1.83mL, and in the most above-mentioned self-made solution, content of formaldehyde is
8.66g/L.It is 866mg that detection obtains adding formaldehyde amount, and actual additional formaldehyde amount is 865.9mg.
Claims (1)
1. one kind is detected the method for content of formaldehyde in alkaline chemical copper plating waste liquid, it is characterised in that include examining as follows
Survey step:
(1) the copper content in Accurate Determining alkaline chemical copper plating waste liquid；
(2) adjust pH ＞ 10, add vulcanized sodium so that copper content is 1:1-5 with the mol ratio of vulcanized sodium, stirring
Make it react, stand and filter；
(3) taking above-mentioned filtrate 50mL, the HCl being slowly added to 5-30wt% regulates pH ＜ 1, and stirring is to nothing
Hydrogen sulfide gas produce, after be settled to 100mL；
(4) take above-mentioned solution 5.00ml, add 10ml 20wt% sodium hydroxide solution；
(5) accurately adding 10.00ml 0.1mol/L iodine standard solution, fluid-tight shakes up, and stands 5-60 in dark place
min；
(6) 10ml 10-30wt% sulfuric acid solution is added；
(7) it is titrated to faint yellow with 0.1mol/L sodium thiosulfate standard solution, adds 2ml 0.5wt% starch
Indicator, continues to drop to blueness and just disappears, and record consumes the volume of sodium thiosulfate standard solution；
(8) it is calculated as follows content of formaldehyde:
Wherein, CI2For iodine mark liquid concentration, mol/L, VI2Amass for iodine mark liquid, ml；CNa2S2O4For sulphur for sulphur
Acid na concn, mol/L；VNa2S2O4For sodium thiosulfate volume, ml；MHCHOFor formaldehyde molal weight,
g/mol；VSample: pipette and treat test sample volume, ml；CHCHOFor content of formaldehyde, g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610208303.1A CN105891201A (en) | 2016-04-05 | 2016-04-05 | Method for detecting content of formaldehyde in alkaline electroless copper plating waste water |
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| CN201610208303.1A CN105891201A (en) | 2016-04-05 | 2016-04-05 | Method for detecting content of formaldehyde in alkaline electroless copper plating waste water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112611749A (en) * | 2020-10-30 | 2021-04-06 | 重庆金美新材料科技有限公司 | Method for detecting content of ammonium citrate in liquid |
| CN114605670A (en) * | 2022-03-28 | 2022-06-10 | 上海时宜品牌管理有限公司 | High-color-difference formaldehyde color-changing hydrogel based on natural pigment |
-
2016
- 2016-04-05 CN CN201610208303.1A patent/CN105891201A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112611749A (en) * | 2020-10-30 | 2021-04-06 | 重庆金美新材料科技有限公司 | Method for detecting content of ammonium citrate in liquid |
| CN114605670A (en) * | 2022-03-28 | 2022-06-10 | 上海时宜品牌管理有限公司 | High-color-difference formaldehyde color-changing hydrogel based on natural pigment |
| CN114605670B (en) * | 2022-03-28 | 2023-12-12 | 上海时宜品牌管理有限公司 | High-chromatic-aberration formaldehyde color-changing hydrogel based on natural pigment |
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Application publication date: 20160824 |