CN101876631A - Method for measuring trace neodymium in industrial wastewater by using spectrophotometer - Google Patents
Method for measuring trace neodymium in industrial wastewater by using spectrophotometer Download PDFInfo
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- CN101876631A CN101876631A CN 201010201301 CN201010201301A CN101876631A CN 101876631 A CN101876631 A CN 101876631A CN 201010201301 CN201010201301 CN 201010201301 CN 201010201301 A CN201010201301 A CN 201010201301A CN 101876631 A CN101876631 A CN 101876631A
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Abstract
The invention relates to a method for measuring trace neodymium in industrial wastewater by using a spectrophotometer. The method comprises the following steps of: 1, drawing standard curves, namely preparing no less than two groups of different standard neodymium solution, and after adding a proper amount of color-developing agent, buffer solution and masking agent sequentially, measuring by using the spectrophotometer and drawing the standard curves of the absorbance and neodymium concentration of the mixture; and 2, measuring trace neodymium in industrial wastewater, namely filtering wastewater to be measured first, after adding the color-developing agent, the buffer solution and the masking agent sequentially, measuring the absorbance of the mixture by using the spectrophotometer, and calculating according to the standard curves obtained in the step 1 to obtain the neodymium content of the wastewater. Through the analysis of the spectrophotometer, the neodymium content of the industrial wastewater is within the range of between 1 and 10 mg/L, and compared with methods of ICP-AES, ICP-MS and the like, the method has the characteristics of quick and convenient measurement, accurate result, simple equipment, strong practicality and the like.
Description
Technical field
The present invention relates to contain the assay method technical field of trace neodymium in the neodymium industrial waste water, is a kind of method with trace neodymium in the spectrophotometric determination factory effluent.
Background technology
In recent years, neodymium element relies on its unique status in the rare earth field, more and more is used widely in correlative technology field.But being paid close attention to more, people contain of the influence of neodymium industrial waste water to environment.Therefore, set up the simple and feasible analytical approach of neodymium in the industrial waste water, the neodymium content in the waste water of enterprise's monitoring generation is necessary and realistic meaning is arranged.But concentrate on the metallurgical analysis of rare earth element at present for the great majority of rare earth neodymium, especially in numerous rare earth element the mensuration of single rare earth element with separate, neodymium Determination on content and research are not seen open report as yet with the method for trace neodymium in the spectrophotometric determination factory effluent.
Summary of the invention
The invention provides a kind of method with trace neodymium in the spectrophotometric determination factory effluent, overcome the deficiency of prior art, it has characteristics such as measurement is quick, convenient, the result is accurate, equipment is fairly simple, practical.
Technical scheme of the present invention is achieved like this: a kind of method with trace neodymium in the spectrophotometric determination factory effluent, it is undertaken by following step: first step drawing standard curve: preparation is no less than two groups different neodymium standard solution, and add successively behind an amount of developer, buffer solution and the screening agent with spectrophotometric determination and draw its absorbance with and the typical curve of neodymium concentration; Trace neodymium in the factory effluent is decided in second pacing: earlier with waste water filtering to be measured, with its absorbance of spectrophotometric determination, calculate the content of neodymium in the waste water again according to the typical curve of first gained after adding developer, buffer solution and screening agent successively.
Be to the further optimization of technique scheme below or/and select:
Above-mentioned spectrophotometer can adopt WFZ800-D3B type single beam ultraviolet/visible spectrophotometer or 722 type spectrophotometers, wavelength 200nm to 800nm, absorbance ∈ [0.041,3.00] Abs.
Above-mentioned developer can adopt the CPA III.
Above-mentioned buffer solution can adopt hydrochloric acid-glycine buffer solution of pH=2.0.
Above-mentioned screening agent can adopt oxalic acid solution.
The above-mentioned method with trace neodymium in the spectrophotometric determination factory effluent can be undertaken by following step:
First step drawing standard curve:
⑴ the preparation of solution:
Neodymium standard solution: accurately take by weighing 0.2916gNd
2O
3In the 100mL beaker, with 10mL to 20mL water-wet, dripping hydrochloric acid is to Nd
2O
3Dissolving fully, heated solution makes excessive hydrochloric acid volatilization, and constant volume is in the 250mL volumetric flask; At this moment, neodymium storing solution concentration is 1000mg/L, pipettes the 5.0mL storing solution in the 500mL volumetric flask, and deionized water is settled to 500mL, gets 10.0mg/L neodymium standard solution;
CPA III ethanolic solution: accurately weighing 0.1250gCPA III adds absolute ethyl alcohol and is settled to 250mL in the 250mL volumetric flask, shakes up, and gets 0.500g/LCPA III ethanolic solution developer;
Buffer solution: take by weighing 1.78gNaCl and 1.95g glycocoll respectively in the 500mL volumetric flask, add 10mL to 20mL deionized water dissolving, add 2.0mL hydrochloric acid again, be settled to 500mL, get hydrochloric acid-glycine buffer solution of pH=2.0;
Screening agent: accurately take by weighing 63.035gC
2H
2O
42H
2O adds the deionized water of 30mL to 40mL in the 50mL beaker, heating for dissolving is transferred in the 250mL volumetric flask, is no less than 3 times with 10mL to 20mL deionized water rinsing beaker, and wash-down water is poured volumetric flask in the lump into, is settled to 250mL at last and obtains the oxalic acid screening agent;
⑵ drawing standard curve
Getting 6 25ml volumetric flask number consecutivelies is: 0
#, 1
#, 2
#, 3
#, 4
#, 5
#, pipette 0,1,2,3,4 respectively, the above-mentioned neodymium standard solution of 5mL, and add above-mentioned 3.0mlCPA III ethanolic solution developer, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively, be settled to 25mL with deionized water; At this moment, the neodymium concentration of solution is respectively 0,0.4,0.8,1.2,1.6 and 2.0mg/L in 6 volumetric flasks;
To the solution in above-mentioned 6 volumetric flasks with spectrophotometric determination its absorbance:
1. the power supply of opening the spectrophotometer instrument carries out preheating, will test wavelength and be adjusted to 674nm; Select the 1cm quartz colorimetric utensil,, stand-by with distilled water flushing to wall built-up not;
2. with 0
#Sample tests 1 as reference successively by the spectrophotometer working specification
#, 2
#, 3
#, 4
#, 5
#Absorbance, and drawing standard curve;
Trace neodymium in the factory effluent is decided in second pacing:
Earlier waste water filtering to be measured is obtained clear filtrate, get 2 25mL volumetric flasks, be numbered 0
#With 1
#, 0
#Middle adding adds 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively as reference, 1
#Add 5mL clear filtrate, 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent in the volumetric flask successively, all be settled to 25mL at last; With 0
#Be reference, measure 1
#The absorbance of sample calculates the content of neodymium in the waste water again according to the typical curve of first gained.
The present invention is with neodymium content is in the scope of 1mg/L to 10mg/L in the spectrophotometer analysis factory effluent, and this and methods such as ICP-AES, ICP-MS compare, and the present invention has characteristics such as measurement is quick, convenient, the result is accurate, equipment is fairly simple, practical.
Description of drawings
Accompanying drawing 1 be the neodymium standard solution absorbance with and the canonical plotting of neodymium concentration.
Embodiment
The present invention is not subjected to the restriction of following most preferred embodiment, can determine concrete embodiment according to technical scheme of the present invention and actual conditions.
Most preferred embodiment of the present invention is as follows:
Adopt absorption photometry to detect the neodymium of trace in the industrial waste water.Developer adopts the CPA III, and spectrophotometer is selected WFZ800-D3B type single beam ultraviolet/visible spectrophotometer (or other model 722 type spectrophotometers), wavelength 200 ~ 800nm, absorbance ∈ [0.041,3.00] Abs for use.
⑴ the preparation of solution
The amount of preparation of following solution can be determined by actual demand.
Nd (III) standard solution: accurately take by weighing 0.2916gNd
2O
3(Nd
2O
3Content 99.9wt%) in the 100mL beaker,, drips (1+1) hydrochloric acid to Nd with 10 ~ 20mL water-wet
2O
3Dissolving fully, heated solution makes excessive hydrochloric acid volatilization, and constant volume is in the 250mL volumetric flask.At this moment, Nd (III) storing solution concentration is 1000mg/L.Pipette the 5.0mL storing solution in the 500mL volumetric flask, deionized water is settled to 500mL, gets 10.0mg/LNd (III) standard solution.
CPA III ethanolic solution: accurately weighing 0.1250gCPA III adds absolute ethyl alcohol and is settled to 250mL in the 250mL volumetric flask, shakes up, and gets 0.500g/LCPA III ethanolic solution.
Buffer solution: take by weighing 1.78gNaCl and 1.95g glycocoll respectively in the 500mL volumetric flask, add 10 ~ 20mL deionized water dissolving, add 2.0mL hydrochloric acid again, be settled to 500mL, get hydrochloric acid-glycine buffer solution of pH=2.0.
Screening agent: accurately take by weighing 63.035gC
2H
2O
42H
2O adds the deionized water of 30 ~ 40mL in the 50mL beaker, heating for dissolving is transferred in the 250mL volumetric flask, repeatedly (is no less than 3 times) with 10 ~ 20mL deionized water rinsing beaker, and wash-down water is poured volumetric flask in the lump into, is settled to 250mL at last.
⑵ drawing standard curve
(the big I of volumetric flask is selected according to actual conditions, adjusts the addition of each reagent by corresponding volume ratio to get 6 25ml volumetric flasks.This operation is an example with the 25mL volumetric flask), number consecutively is: 0
#, 1
#, 2
#, 3
#, 4
#, 5
#, pipette 0,1,2,3,4 respectively, Nd (III) standard solution of 5mL, and add 3.0mlCPA III ethanolic solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL screening agent successively, be settled to 25mL with deionized water.At this moment, Nd (III) concentration in 6 volumetric flasks is respectively 0,0.4,0.8,1.2,1.6 and 2.0mg/L.
Next carry out as follows:
1. open the spectrophotometer power supply, preheating will be tested wavelength and be adjusted to 674nm; Select the 1cm quartz colorimetric utensil,, stand-by with distilled water flushing to wall built-up not;
2. with 0
#Sample tests 1 as reference successively by the spectrophotometer working specification
#, 2
#, 3
#, 4
#, 5
#Absorbance, and drawing standard curve such as Fig. 1 (method for drafting of typical curve: adopt principle of least square method to fit to straight line (y=kx) absorbance (ordinate y) and Nd (III) concentration (horizontal ordinate x).If coefficient of multiple correlation R
2〉=0.99, then typical curve is drawn successfully, and this moment, slope of a curve was k.）
⑶ the checking of typical curve
Get 3 25mL volumetric flasks, be numbered a1
#, a2
#And a3
#, Nd (III) standard solution that pipettes 1.5mL, 2.5mL and 3.5mL respectively adds 3.0mlCPA III ethanolic solution and 9.0mL hydrochloric acid-glycine buffer solution successively in volumetric flask, be settled to the 25mL scale mark with deionized water.The absorbance that records the 674nm place successively is respectively 0.240,0.402 and 0.581, relative error be respectively 2.30%, 2.81% and-1.43%(relative error ∈ [3,3] %), typical curve can use.
⑷ measure the neodymium content in the water sample
Earlier with waste water filtering to be measured, it is stand-by in beaker to get the 100mL clear filtrate.Get 2 25mL volumetric flasks, be numbered 0
#With 1
#, 0
#Middle adding adds 3.0mlCPA III ethanolic solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL screening agent successively as reference, 1
#Add 5mL clear filtrate, 3.0mlCPA III ethanolic solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL screening agent in the volumetric flask successively, all be settled to 25mL at last.
With 0
#Be reference, measure 1
#The absorbance of sample is the then dense c(mg/L of Nd (III) in the water sample of A) computing formula is: c=(5A)/k(k is the slope of typical curve).
By table 1 as can be known: the present invention not only analyzes in the factory effluent neodymium content in the scope of 1～10mg/L with spectrophotometer, and with methods such as ICP-AES, ICP-MS relatively, its have measure fast, convenient, the result is accurate, equipment is fairly simple, characteristics such as practical.
Claims (9)
1. method with trace neodymium in the spectrophotometric determination factory effluent is characterized in that being undertaken by following step:
First step drawing standard curve: preparation is no less than two groups different neodymium standard solution, and add successively behind an amount of developer, buffer solution and the screening agent with spectrophotometric determination and draw its absorbance with and the typical curve of neodymium concentration;
Trace neodymium in the factory effluent is decided in second pacing: earlier with waste water filtering to be measured, with its absorbance of spectrophotometric determination, calculate the content of neodymium in the waste water again according to the typical curve of first gained after adding developer, buffer solution and screening agent successively.
2. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 1, it is characterized in that spectrophotometer adopts WFZ800-D3B type single beam ultraviolet/visible spectrophotometer or 722 type spectrophotometers, wavelength 200nm to 800nm, absorbance ∈ [0.041,3.00] Abs.
3. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 1 and 2 is characterized in that developer adopts the CPA III.
4. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 1 and 2 is characterized in that buffer solution adopts hydrochloric acid-glycine buffer solution of pH=2.0.
5. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 3 is characterized in that buffer solution adopts hydrochloric acid-glycine buffer solution of pH=2.0.
6. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 1 and 2 is characterized in that screening agent adopts oxalic acid solution.
7. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 5 is characterized in that screening agent adopts oxalic acid solution.
8. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 1 and 2 is characterized in that being undertaken by following step:
First step drawing standard curve:
⑴ the preparation of solution:
Neodymium standard solution: accurately take by weighing 0.2916gNd
2O
3In the 100mL beaker, with 10mL to 20mL water-wet, dripping hydrochloric acid is to Nd
2O
3Dissolving fully, heated solution makes excessive hydrochloric acid volatilization, and constant volume is in the 250mL volumetric flask; At this moment, neodymium storing solution concentration is 1000mg/L, pipettes the 5.0mL storing solution in the 500mL volumetric flask, and deionized water is settled to 500mL, gets 10.0mg/L neodymium standard solution;
CPA III ethanolic solution: accurately weighing 0.1250gCPA III adds absolute ethyl alcohol and is settled to 250mL in the 250mL volumetric flask, shakes up, and gets 0.500g/LCPA III ethanolic solution developer;
Buffer solution: take by weighing 1.78gNaCl and 1.95g glycocoll respectively in the 500mL volumetric flask, add 10mL to 20mL deionized water dissolving, add 2.0mL hydrochloric acid again, be settled to 500mL, get hydrochloric acid-glycine buffer solution of pH=2.0;
Screening agent: accurately take by weighing 63.035gC
2H
2O
42H
2O adds the deionized water of 30mL to 40mL in the 50mL beaker, heating for dissolving is transferred in the 250mL volumetric flask, is no less than 3 times with 10mL to 20mL deionized water rinsing beaker, and wash-down water is poured volumetric flask in the lump into, is settled to 250mL at last and obtains the oxalic acid screening agent;
⑵ drawing standard curve
Getting 6 25ml volumetric flask number consecutivelies is: 0
#, 1
#, 2
#, 3
#, 4
#, 5
#, pipette 0,1,2,3,4 respectively, the above-mentioned neodymium standard solution of 5mL, and add above-mentioned 3.0mlCPA III ethanolic solution developer, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively, be settled to 25mL with deionized water; At this moment, the neodymium concentration of solution is respectively 0,0.4,0.8,1.2,1.6 and 2.0mg/L in 6 volumetric flasks;
To the solution in above-mentioned 6 volumetric flasks with spectrophotometric determination its absorbance:
1. the power supply of opening the spectrophotometer instrument carries out preheating, will test wavelength and be adjusted to 674nm; Select the 1cm quartz colorimetric utensil,, stand-by with distilled water flushing to wall built-up not;
2. with 0
#Sample tests 1 as reference successively by the spectrophotometer working specification
#, 2
#, 3
#, 4
#, 5
#Absorbance, and drawing standard curve;
Trace neodymium in the factory effluent is decided in second pacing:
Earlier waste water filtering to be measured is obtained clear filtrate, get 2 25mL volumetric flasks, be numbered 0
#With 1
#, 0
#Middle adding adds 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively as reference, 1
#Add 5mL clear filtrate, 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent in the volumetric flask successively, all be settled to 25mL at last; With 0
#Be reference, measure 1
#The absorbance of sample calculates the content of neodymium in the waste water again according to the typical curve of first gained.
9. the method with trace neodymium in the spectrophotometric determination factory effluent according to claim 7 is characterized in that being undertaken by following step:
First step drawing standard curve:
⑴ the preparation of solution:
Neodymium standard solution: accurately take by weighing 0.2916gNd
2O
3In the 100mL beaker, with 10mL to 20mL water-wet, dripping hydrochloric acid is to Nd
2O
3Dissolving fully, heated solution makes excessive hydrochloric acid volatilization, and constant volume is in the 250mL volumetric flask; At this moment, neodymium storing solution concentration is 1000mg/L, pipettes the 5.0mL storing solution in the 500mL volumetric flask, and deionized water is settled to 500mL, gets 10.0mg/L neodymium standard solution;
CPA III ethanolic solution: accurately weighing 0.1250gCPA III adds absolute ethyl alcohol and is settled to 250mL in the 250mL volumetric flask, shakes up, and gets 0.500g/LCPA III ethanolic solution developer;
Buffer solution: take by weighing 1.78gNaCl and 1.95g glycocoll respectively in the 500mL volumetric flask, add 10mL to 20mL deionized water dissolving, add 2.0mL hydrochloric acid again, be settled to 500mL, get hydrochloric acid-glycine buffer solution of pH=2.0;
Screening agent: accurately take by weighing 63.035gC
2H
2O
42H
2O adds the deionized water of 30mL to 40mL in the 50mL beaker, heating for dissolving is transferred in the 250mL volumetric flask, is no less than 3 times with 10mL to 20mL deionized water rinsing beaker, and wash-down water is poured volumetric flask in the lump into, is settled to 250mL at last and obtains the oxalic acid screening agent;
⑵ drawing standard curve
Getting 6 25ml volumetric flask number consecutivelies is: 0
#, 1
#, 2
#, 3
#, 4
#, 5
#, pipette 0,1,2,3,4 respectively, the above-mentioned neodymium standard solution of 5mL, and add above-mentioned 3.0mlCPA III ethanolic solution developer, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively, be settled to 25mL with deionized water; At this moment, the neodymium concentration of solution is respectively 0,0.4,0.8,1.2,1.6 and 2.0mg/L in 6 volumetric flasks;
To the solution in above-mentioned 6 volumetric flasks with spectrophotometric determination its absorbance:
1. the power supply of opening the spectrophotometer instrument carries out preheating, will test wavelength and be adjusted to 674nm; Select the 1cm quartz colorimetric utensil,, stand-by with distilled water flushing to wall built-up not;
2. with 0
#Sample tests 1 as reference successively by the spectrophotometer working specification
#, 2
#, 3
#, 4
#, 5
#Absorbance, and drawing standard curve;
Trace neodymium in the factory effluent is decided in second pacing:
Earlier waste water filtering to be measured is obtained clear filtrate, get 2 25mL volumetric flasks, be numbered 0
#With 1
#, 0
#Middle adding adds 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent successively as reference, 1
#Add 5mL clear filtrate, 3.0mlCPA III ethanol chromogenic reagent solution, 9.0mL hydrochloric acid-glycine buffer solution and 5mL oxalic acid screening agent in the volumetric flask successively, all be settled to 25mL at last; With 0
#Be reference, measure 1
#The absorbance of sample calculates the content of neodymium in the waste water again according to the typical curve of first gained.
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|---|---|---|---|
| CN2010102013012A CN101876631B (en) | 2010-06-17 | 2010-06-17 | Method for measuring trace neodymium in industrial wastewater by using spectrophotometer |
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|---|---|---|---|
| CN2010102013012A CN101876631B (en) | 2010-06-17 | 2010-06-17 | Method for measuring trace neodymium in industrial wastewater by using spectrophotometer |
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| CN101876631B CN101876631B (en) | 2012-05-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486651A (en) * | 2016-01-21 | 2016-04-13 | 湖北金洋冶金股份有限公司 | Chemical analysis method of lanthanum in lead-base alloy |
| CN111707627A (en) * | 2020-06-30 | 2020-09-25 | 武汉钢铁有限公司 | Rapid analysis method for nitrate radical in reusable metallurgical waste ammonia water |
| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036293C (en) * | 1994-03-21 | 1997-10-29 | 颜炳玉 | Device for non-destructive inspection of neodymium distributed gradient in yttrium aluminium garnet laser crystal |
| CN1117980C (en) * | 1999-11-26 | 2003-08-13 | 中国科学院地质与地球物理研究所 | One-step mass spectrographic analysis process to measure the ratio and contents of neodymium isotopes |
-
2010
- 2010-06-17 CN CN2010102013012A patent/CN101876631B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036293C (en) * | 1994-03-21 | 1997-10-29 | 颜炳玉 | Device for non-destructive inspection of neodymium distributed gradient in yttrium aluminium garnet laser crystal |
| CN1117980C (en) * | 1999-11-26 | 2003-08-13 | 中国科学院地质与地球物理研究所 | One-step mass spectrographic analysis process to measure the ratio and contents of neodymium isotopes |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486651A (en) * | 2016-01-21 | 2016-04-13 | 湖北金洋冶金股份有限公司 | Chemical analysis method of lanthanum in lead-base alloy |
| CN105486651B (en) * | 2016-01-21 | 2018-06-05 | 湖北金洋冶金股份有限公司 | The chemical analysis method of lanthanum in a kind of lead-containing alloy |
| CN111707627A (en) * | 2020-06-30 | 2020-09-25 | 武汉钢铁有限公司 | Rapid analysis method for nitrate radical in reusable metallurgical waste ammonia water |
| CN111707627B (en) * | 2020-06-30 | 2023-03-31 | 武汉钢铁有限公司 | Rapid analysis method for nitrate radical in reusable metallurgical waste ammonia water |
| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
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|---|---|
| CN101876631B (en) | 2012-05-30 |
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Application publication date: 20101103 Assignee: XINJIANG DE MEI LONG SYNTHETIC MATERIAL TECHNOLOGY CO., LTD. Assignor: Xinjiang University Contract record no.: 2015650000010 Denomination of invention: Method for measuring trace neodymium in industrial wastewater by using spectrophotometer Granted publication date: 20120530 License type: Exclusive License Record date: 20150311 |
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