CN108760654A - A kind of method of lead element content in quick measurement tin plate coating - Google Patents
A kind of method of lead element content in quick measurement tin plate coating Download PDFInfo
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- CN108760654A CN108760654A CN201810400985.5A CN201810400985A CN108760654A CN 108760654 A CN108760654 A CN 108760654A CN 201810400985 A CN201810400985 A CN 201810400985A CN 108760654 A CN108760654 A CN 108760654A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3196—Correlating located peaks in spectrum with reference data, e.g. fingerprint data
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Abstract
The invention discloses a kind of methods of lead element content in quick measurement tin plate coating.The method that the present invention quickly measures lead element content in tin plate coating includes (1) sample pre-treatments；(2) it is electrolysed detin；(3) preparing standard solution comprising the preparation of lead standard solution, matrix modifier and dilution；(4) lead element measures.This method only needs to make a sample, and detection time is short, efficient, and accuracy is high.
Description
Technical field
The present invention provides a kind of methods of lead element content in quick measurement tin plate coating, especially a kind of to use stone
The method that black stove Atomic absorption quickly directly measures lead element content in coating electrolyte, belongs to detection technique field.
Background technology
The tin plate being packed for for food and beverage in European Union BS EN 10333-2005, which proposes, to be clearly required, plating
Lead content in layer is less than 100ppm.Therefore tin plate needs to monitor the lead content in coating in real time in process of production, also
It is that the lead content in tin plate coating is needed to be included in the detection of tin plate Quality Process.
The measurement of lead content in the tin plate coating provided in European Union's BS EN 10333-2005 appendix As is to use coulomb method
Tin coating is dissolved down, hydrobromic acid is added and removes the tin crossed in electrolyte, then uses the lead in atomic absorption detecting solution
Content.It must be driven off the tin in solution in this method operating process, the sulfuric acid being added in electrolyte is also burnt, before sample
Reason process is complicated, long flow path, and the electrolyte sample for preparing a print just needs 4-6 hours, cannot be satisfied produced on-site detection
Demand.
The assay method in industry about lead content in tin plate coating has the following problems at present：1) measurement accuracy is low,
The detection of the more coating lead content in industry includes inductively coupled plasma atomic emission spectrometry and X-ray at present
Fluorescent spectrometry.First method directly detects the solution after stripping with ICP, does not account for shadow of the interference element to lead
It rings；The problem of second method is to measure lead content in coating using fundamental parameters method (FP), this method is that X-ray is bound to
The lead being mapped in substrate, and lead content in substrate is nor fixed value, especially when substrate thickness is less than 0.2mm due to X
Ray projects the another side of tin plate, and the testing result of the method can have obvious deviation；2) time for sample pretreatment is long, electricity
Sense coupled plasma-atomic emission spectrometry needs electrolytic sample 5-10 blocks, and needs electrolyte is dense on electric boiling plate
It is reduced to 10ml, long flow path, detection efficiency is low；3) applicable measurement range is indefinite.It is mentioned in European Union BS EN 10333-2005,
Lead content is more than 2.8g/m in the corresponding thickness of coating of 0-100 μ g/L in coating stripping solution2, but without clearly corresponding
The scope of application of coating lead content.The standard requires lead content in coating to be less than 100ppm, but lead content is lower to be more difficult to detect,
The coating lead content range encountered in actually detected at present is about 20ppm-300ppm, and actual range span is big and does not mark
Quasi- sample, accuracy in detection can not ensure.
Invention content
The present invention provides a kind of methods of lead element content in quick measurement tin plate coating, it is intended to solve existing detection
The problem that method detection time is long, accuracy of detection is low, Matrix effects are big.
The present invention relates to a kind of methods of lead element content in quick measurement tin plate coating, it is characterised in that：This method
Include the following steps：
(1) sample pre-treatments；
(2) it is electrolysed detin；
(3) preparing standard solution comprising the preparation of lead standard solution, matrix modifier and dilution；
(4) lead element measures.
It is prepared in the quick measurement tin plate coating in certain specific embodiments of lead element content in the present invention,
Step is recorded twice the potential break time in (2)：The time T of pure stannum layer electrolysis stripping1And pure stannum layer is shelled with alloy-layer electrolysis
From total time TAlways。
It is prepared in the quick measurement tin plate coating in certain specific embodiments of lead element content in the present invention,
A concentration of 15 μ g/L of lead standard solution described in step (3).
It is prepared in the quick measurement tin plate coating in certain specific embodiments of lead element content in the present invention,
Matrix modifier described in step (3) is the mixed solution of diammonium hydrogen phosphate, magnesium nitrate and nitric acid.
Further, the mass fraction of diammonium hydrogen phosphate, nitric acid and magnesium nitrate is 1: 2 in the mixed solution:
0.06。
It is prepared in the quick measurement tin plate coating in certain specific embodiments of lead element content in the present invention,
Dilution described in step (3) is salpeter solution.
Further, a concentration of the 2% of the dilution.
It is prepared in the quick measurement tin plate coating in certain specific embodiments of lead element content in the present invention,
The lead element in lead standard solution and sample solution is measured using sampling Graphite Furnace Atomic Absorption in step (4), and examination is calculated as follows
Lead content in sample：
Tin plating time T=T1(free tin time)+2 × (TAlways-T1) (alloy tin time)/3 (1)
Coating weight (mg)=Area of Sample (cm2)×T×119/2/96500 (2)
Lead content/sample coating weight (3) in coating lead content=sample coating
T1：The time of pure stannum layer electrolysis stripping, unit s；
TAlways：The total time of pure stannum layer and alloy-layer electrolysis stripping, unit S；
Coating lead content：Unit is ppm, is as a result retained to integer-bit；
Lead content in sample coating：Unit is μ g；
Sample coating weight：Unit is mg.
The present invention measures the test method of lead standard solution and the lead element in sample solution using sampling Graphite Furnace Atomic Absorption
It is as follows：Equipment self-inspection, preheating collimation sample introduction needle after the completion are opened, graphite-pipe can be entered three times and all in centre position ability
Start to detect；Lead standard solution, matrix modifier, blank solution, dilution, sample are put well according to sequence, start to measure, equipment
10 times, lead standard solution dilution 2 times, lead standard solution are diluted according to blank solution, lead standard solution, to each solution detection two
All over standard curve is drawn out, then measures the signal strength of lead element in sample and bring into standard curve, calculate sample plating
Lead content in layer.
Embodiment 1
In order to better understand the above technical scheme, being done in detail to above-mentioned technical proposal below in conjunction with specific embodiment
Thin explanation.
Shown in reagent and raw material following article table 1 used in the present invention：
1 reagent used in the present invention of table and raw material
Instrument：
It is electrolysed the instrument of detin：Electrochemical workstation, Shanghai Chen Hua instrument CHI760E
The setting of experiment condition：Chronoptentiometry is chosen, parameter is set as Cathodic Current 0.005A,
Anodic Current 0.24A, Cathodic Time 0.005s, Anodic Time 300s, Initial Polarity
Anodic。
Measure the instrument of lead element：Graphite furnace atomic absorption spectrophotometer, THERMO FISHER SCIENTIFIC,
ICE3300
The setting of experiment condition：Wavelength 217nm, lamp current 10A, spectral band-width width 0.5nm, 15 μ L of sampling volume, phosphorus
Sour 5 μ L of hydrogen diammonium-magnesium nitrate Matrix modifier, carrier gas are argon gas, air-flow 0.2L/min, mensuration mode peak height, background school
Positive four lines deuterium lamp.
Graphite furnace temperature program：It is 100 DEG C dry, it is kept for 30 seconds, 10 DEG C/sec of slope；850 DEG C of ashing is kept for 20 seconds, slope
150 DEG C/sec；2000 DEG C of atomization is kept for 3 seconds；2500 DEG C are removed, is kept for 3 seconds.
The method of lead element content includes in a kind of quick measurement tin plate coating of the present invention：
S1：Sample pre-treatments
Sample A is cut into one piece of A4 (210mm × 297mm) sample；In model non-detection face reel number rule are filled in marking pen
Lattice and coating information simultaneously paste side edge and make a call to 3 lattice, and size is 30 × 110mm；With scraper in the uniform rod coating supernatant in non-detection face
Paint PPG 6305-301/A/200K-C4 are closed, and are then placed in the baking oven that set temperature is 185 DEG C and are toasted 10 minutes, take
Go out cooling；The small print that model after baking is accurately cut to one piece of 30 × 110mm along scribing line, then again in 30 × 100mm
Place, which cuts off only to stay not cut, is used for connection electrode, other remainders keep sample as sample is reviewed；Alcohol is dipped with absorbent cotton
It is the small print two sides 30 × 100mm is clean and dry, print is then bent into cylinder along long side direction, face to be detected exists
It is interior.
S2：It is electrolysed detin
The sample for bending to cylinder is put into 50ml beakers, sample connects working electrode, and platinum filament connects auxiliary electrode, calomel electricity
Pole connects reference electrode；Electrochemical operation station software is opened, confirms and selects chronoptentiometry, anode current is set as 0.24A, and really
It is good to recognize electrode connection；Auxiliary electrode and reference electrode are placed on to the center location of cylinder sample；2mol/ is added in beaker
The hydrochloric acid solution of L did not had electrode just, clicks at once and starts detin, and second potential break point stops electrolysis, record after occurring
The time T1 of potential break time twice, pure stannum layer electrolysis stripping are 13.0s, the total time of pure stannum layer and alloy-layer electrolysis stripping
T is always 26.9s；Print and electrode are taken out, electrolyte is poured into 500ml volumetric flasks, then uses deionized water lavage specimens piece, electricity
Pole and beaker pour into 500ml volumetric flasks for each 3 times, and constant volume in 500ml volumetric flasks is added in the nitric acid of 50ml 20%, completes tin
It is prepared by layer electrolyte.
S3：Standard solution is prepared
Lead standard solution：The lead standard solution 1ml for taking 1000mg/L, pours into constant volume in the volumetric flask of 100ml, concentration dilution
For 10mg/L；Take the above-mentioned solution of 5ml that constant volume in 100ml volumetric flasks, concentration dilution 0.5mg/L is added；Take the above-mentioned solution of 3ml
It is added in 100ml volumetric flasks, adds constant volume after the salpeter solution of 10ml 20%, concentration dilution is that the preceding standard of 15 μ g/L is molten
Liquid；
Matrix modifier：Diammonium hydrogen phosphate 1g is put into 100ml beakers, 30ml distillation water dissolutions are added, adds 10ml
20% nitric acid adds magnesium nitrate 60mg, and candidate agent dissolving is complete, moves into 100ml volumetric flasks, constant volume；
Dilution measures 20ml nitric acid and constant volume in the volumetric flask of 1000ml is added, obtains 2% salpeter solution.
S4：Lead element measures
Lead element in lead standard solution and sample solution is measured using sampling Graphite Furnace Atomic Absorption, and calculates the lead in sample
Content：Equipment self-inspection, preheating collimation sample introduction needle after the completion are opened, graphite-pipe can be entered three times and all in centre position ability
Start to detect；Lead standard solution, matrix modifier, blank solution, dilution, sample are put well according to sequence, start to measure, equipment
Twice is detected to each solution and draws out standard curve, curve matching 0.9999 measures the absorption peak 0.270 of lead element in sample
For and bring into standard curve, it is 0.34 μ g, RSD 1.2% to calculate lead content in sample coating；
1) tin plating time T=T1(free tin time)+2 × (TAlways-T1) (alloy tin time) ÷ 3=22.27 S
2) coating weight (mg)=8 × 30 (Area of Sample, cm2) × T × 119/2/96500=3.295mg
3) lead content/sample coating weight=0.34/3.295*1000=102 ppm in coating lead content=sample coating
Mark-on reclaims verify the measurement result of the present embodiment sample absorbance, and the mark-on knot of three different levels is done to sample
Fruit is as shown in table 2, it can be seen that this method to the recovery of standard addition of lead content in coating between 95.05%-103.59%,
It is 3.24%, 2.89% repeatedly to measure RSD, it is seen that it is sensitive and accurate that lead is measured under the present embodiment method.
2 sample recovery of standard addition measurement result of table
Comparative example 1
Standard solution, dilution, sample electrolyte are same as Example 1, and difference lies in matrix modifiers only to add 60mg
Magnesium nitrate and 10ml 20% nitric acid, be not added with diammonium hydrogen phosphate；
The experiment condition setting of sampling Graphite Furnace Atomic Absorption is measured with embodiment 1 in lead standard solution and tin layers electrolyte
Lead element, curve matching 0.9999, the absorption peak for then measuring lead element in sample twice is respectively 0.136 and 0.102,
RSD is 14.29%, and absorption peak is relatively low, and poor repeatability experimental result is undesirable.
Technical solution in the embodiment of the present application has at least the following technical effects or advantages：
1) method for utilizing company's existing equipment to research and develop lead element content in a kind of quick detection tin plate coating is company
Save equipment purchase fund.
2) this method only needs to make a sample, and detection time is short, efficient；
3) sampling Graphite Furnace Atomic Absorption high sensitivity, detection are limited to ppb grades, are more suitable for the accurate survey of single Determination of trace element contents
It is fixed；
4) hydrochloric acid of electrolysis is high purity reagent in this method, does not bring impurity lead into；
5) the coating weight of sample is measured in this method according to the coulomb method in national standard ferrostan tin coating weight test method
Amount, accuracy are high；
6) it is mainly a large amount of tin element and ferro element and other trace meters in electrolyte sample made from this method
Element, lead element to be measured are trace element, and Matrix effects are big, by adding suitable matrix modifier and with without member to be measured
The Matrix Solution of element carrys out correcting background absorption, and accuracy is high.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.Obviously, those skilled in the art can be to the present invention
Carry out various modification and variations without departing from the spirit and scope of the present invention.If in this way, these modifications and changes of the present invention
Within the scope of the claims of the present invention and its equivalent technology, then the present invention is also intended to exist comprising these modification and variations
It is interior.
Claims (8)
1. a kind of method of lead element content in quick measurement tin plate coating, which is characterized in that the method includes following steps
Suddenly：
(1) sample pre-treatments；
(2) it is electrolysed detin；
(3) preparing standard solution comprising the preparation of lead standard solution, matrix modifier and dilution；
(4) lead element measures.
2. the method for quickly measuring lead element content in tin plate coating as described in claim 1, which is characterized in that in step
(2) the potential break time is recorded twice in：The time T of pure stannum layer electrolysis stripping1And the pure stannum layer is shelled with alloy-layer electrolysis
From total time TAlways。
3. the method for quickly measuring lead element content in tin plate coating as described in claim 1, which is characterized in that step (3)
Described in lead standard solution a concentration of 15 μ g/L.
4. the method for quickly measuring lead element content in tin plate coating as described in claim 1, which is characterized in that step (3)
Described in matrix modifier be diammonium hydrogen phosphate, magnesium nitrate and nitric acid mixed solution.
5. the method for quickly measuring lead element content in tin plate coating as claimed in claim 4, which is characterized in that the mixing
The mass fraction of diammonium hydrogen phosphate, nitric acid and magnesium nitrate is 1 in solution:2:0.06.
6. the method for quickly measuring lead element content in tin plate coating as described in claim 1, which is characterized in that step (3)
Described in dilution be salpeter solution.
7. the method for quickly measuring lead element content in tin plate coating as claimed in claim 6, which is characterized in that the nitric acid
A concentration of the 2% of solution.
8. the method for lead element content in a kind of quick measurement tin plate coating as described in claim 1, which is characterized in that
The lead element in lead standard solution and sample solution is measured using sampling Graphite Furnace Atomic Absorption in step (4), and examination is calculated as follows
Lead content in sample：
Tin plating time T=T1(free tin time)+2 × (TAlways-T1) (alloy tin time)/3
Coating weight (mg)=Area of Sample (cm2) × T × 119/2/96500
Lead content/sample coating weight in coating lead content=sample coating
Wherein：
T1:The time of pure stannum layer electrolysis stripping, unit S；
TAlways:The total time of pure stannum layer and alloy-layer electrolysis stripping, unit S；
Coating lead content：Unit is ppm, is as a result retained to integer-bit；
Lead content in sample coating：Unit is μ g；
Sample coating weight：Unit is mg.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111077267A (en) * | 2020-01-14 | 2020-04-28 | 东莞东阳光科研发有限公司 | Method for measuring lead content in electronic optical foil |
| CN117907562A (en) * | 2024-03-19 | 2024-04-19 | 张家港扬子江冷轧板有限公司 | Method for simultaneously detecting contents of multiple elements in coating |
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| CN117907562A (en) * | 2024-03-19 | 2024-04-19 | 张家港扬子江冷轧板有限公司 | Method for simultaneously detecting contents of multiple elements in coating |
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