CN108344731A - A kind of detection method for measuring quantity of cadmium release in domestic ceramics - Google Patents
A kind of detection method for measuring quantity of cadmium release in domestic ceramics Download PDFInfo
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Abstract
The invention discloses one kind for measuring quantity of cadmium release detection method in domestic ceramics, and this method includes 1, cleans domestic ceramics sample to be measured, and naturally dry；2, wiping agent is dipped with test paper, and test paper is folded, be close to domestic ceramics surface, carry out horizontal and vertical wiping；3, the test paper wiped is placed on colour plate, color developing agent in drop, is stood, under bright light condition, compareed card with cadmium standard work color range and compareed, the range of results of cadmium wiping amount in sample is determined with optical colorimetry；4, quantity of cadmium release is obtained by cadmium wiping amount and stripping quantity linear equation.Compared with the prior art, the present invention has the advantages of：The detection of cadmium is limited to 10ng, entire to analyze 5~10min of test process, greatly shortens analysis time, improves working efficiency.This method have it is easy, quick, easy to operate, disclosure satisfy that the requirement that quantity of cadmium release is quickly analyzed in domestic ceramics.
Description
Technical field
The present invention relates to the detection method technical fields of ceramic product chemical composition, in particular to one kind is used for
Measure quantity of cadmium release detection method in domestic ceramics.
Background technology
Domestic ceramics is daily necessities indispensable in daily life, has many people that can select to be decorated with beautiful muffle painting
Domestic ceramics etc. holds food.Domestic ceramics heavy metal stripping quantity detection in recent years is not used in qualification rate 2 ‰ or so, but by
3 working days are needed in test in laboratory, relatively long detection cycle reduces the clearance speed of inlet and outlet product, import
Quotient may need the port outside amount paid to keep in expense.
On the one hand the demand sternly supervised is needed, is on the other hand the necessity for promoting detection speed, in order to solve these
Problem needs one kind quickly, easy, is intuitively solved with the quick screening method of quantity of cadmium release in sensitive domestic ceramics.
There is the risk main source containing cadmium in domestic ceramics：The pigment used on domestic ceramics.Colored drawing domestic ceramics is divided into
Three kinds of overglaze color, in-glaze decoration and underglaze colour do not take off in order to enable bright in colour, this kind of pigment be added to mostly a large amount of lead, cadmium,
The harmful elements such as mercury, chromium.Underglaze colour, the pigment on in-glaze decoration class ceramic, harmful element therein can not be molten by glaze closing
Go out, so it is safer, and overglaze color based article is outer since pigment is exposed to substantially, there are the risks of cadmium dissolution.
Currently, the national standard in China is to the detection method of quantity of cadmium release in domestic ceramics《It uses within GB/T3534-2002 days
The assay method of ware lead, quantity of cadmium release》, impregnated 24 hours at 22 ± 2 DEG C using 4% acetum, reuse atom
Absorption spectrometer or inductively coupled plasma emission spectrography test quantity of cadmium release in daily ceramics sample.Entire experiment week
Phase generally takes three days, and detection cycle is partially long.
Cadmium belongs to subgroup element in periodic table, and there are many elements similar with its character can be dry to its colour developing generation
It disturbs, the member that interference can be generated in the process color of cadmium is known as V, Zn, Co, Ni, Mn, Cu etc., due to subgroup element character class
Seemingly, the phenanthroline that can shelter the interference elements such as Co well, also has Cd same masking effect.Other screening agents are such as
EDTA etc. also has same problem.And thiocarbamide is less than Cu to the competition performance of Cu, causes the interference of Cu that can not similarly remove.
The present inventor is directed to the above situation, by constantly studying, develops a kind of for quickly detecting in domestic ceramics
The kit of quantity of cadmium release, and specific detection method is had studied, it has broad application prospects.
Invention content
The technical problems to be solved by the invention are exactly insufficient present in current detection method in order to overcome, it is proposed that one
Detection method of the kind for measuring quantity of cadmium release in domestic ceramics, relative to existing detection method, detection method of the invention
Speed is faster, it can be achieved that quickly detection.
In order to solve the above technical problems, present invention employs technical solutions below to come：This is used to measure in domestic ceramics
The detection method of quantity of cadmium release, this method are needed using test paper, wiping agent, color developing agent, colour plate and cadmium standard work color
Rank is blocked, wherein the wiping agent is mixed phosphate salt buffer, a concentration of 1mol/L, pH 9.0；The color developing agent is served as reasons
Mixed aqueous solution includes according to weight percent：Cadion 0.02%, sodium chloride 0.05%, thiocarbamide 2%, chromogenic reagent solution
PH is 9.0；The cadmium standard works color scale card within the scope of 0~100ng；When test, the first step, by domestic ceramics sample to be measured
Product are cleaned, and naturally dry；Second step dips wiping agent with test paper, and test paper is folded, and is close to domestic ceramics surface,
Carry out horizontal and vertical wiping；Third walks, and the test paper wiped is placed on colour plate, color developing agent in drop, stands, bright
Light condition under, compare card with cadmium standard work color range and compareed, cadmium wiping amount in sample is determined with optical colorimetry
Range of results；4th step obtains quantity of cadmium release by cadmium wiping amount and stripping quantity linear equation, which is：Y=
0.024x+0.074, wherein x are cadmium wiping amount, and unit ng, y are quantity of cadmium release, unit mg.
Furthermore, in above-mentioned technical proposal, the test paper is dustless quantitative test paper, and the colour plate is white plastic
Plate.
Furthermore, in above-mentioned technical proposal, the wiping agent preparation method is：According to dipotassium hydrogen phosphate and phosphoric acid
Potassium dihydrogen is according to 5.29：0.41 weight ratio configures aqueous solution, and 0.1mol/L sodium hydroxide solution tune is used in combination in a concentration of 1mol/L
It is 9.0 to pH value.
Furthermore, in above-mentioned technical proposal, cadion uses p-nitrophenyl diazoamino azo in the color developing agent
Benzene, and it is formulated in 0.1mol/L NaOH ethanol solutions.
Furthermore, in above-mentioned technical proposal, in the second step, test paper is first subjected to 4 refoldings before wiping, tightly
Domestic ceramics surface is pasted, first laterally wiping 8 times, then by the wiping surface of test paper reflexed inwardly, is close to domestic ceramics surface, it is longitudinal to wipe
It wipes 8 times.
Furthermore, in above-mentioned technical proposal, the chromogenic reagent solution pH is 9.0, determines chromogenic reagent solution pH's
Method is：0.2g cadions are taken, the ethanol solution of 0.2mol/LNaOH, and constant volume 100mL are dissolved in, as cadion storing solution；
The Triton-X100 aqueous solutions of 10% (V/V) are prepared simultaneously；
5mL cadion storing solutions are added in 50mL volumetric flasks, 400 μ L cadmium standard solution are added, 100 μ L's 10%
Triton-X100 aqueous solutions carry out wavelength full scan analysis with ultraviolet specrophotometer, and scanning range is 300nm~650nm,
And the pH value for adjusting solution is respectively 5.0,6.5,7.0,8.5,9.0,10,11 and 12, all-wave length is swept under above-mentioned pH value respectively
It retouches；
It is obtained according to scanning result：When pH value is more than 8.0, cadmium is combined apparent enhancing, cadion to absorb with cadion
There is an acromion and is gradually increasing at 475nm in curve, while main absorption peak reduces, and solution colour becomes red from orange；
And pH be more than after 11 cadion occur absorption peak at 553nm, itself become aubergine, so pH when cadion measures cadmium is answered
More than 8, while being less than 11, final optimization pass confirms that chromogenic reagent solution pH is 9.0.
Furthermore, in above-mentioned technical proposal, the cadmium wiping amount and the confirmation method of stripping quantity linear equation are：
It is research object to select the white disk of domestic ceramics, coats a series of simulation pigment of cadmiums containing various concentration in Bai Panshang respectively, is carried out
Wipe test and stripping quantity experiment, and wiping amount and stripping quantity are recorded, then calculate the linear relationship of the two.
Furthermore, in above-mentioned technical proposal, in the confirmation method of the cadmium wiping amount and stripping quantity linear equation,
The simulation pigment is using boric acid, sodium chloride, calcium nitrate and basic magnesium carbonate as matrix；Above-mentioned mixing salt is added to coating
In after stir evenly, as bottom material, then be mixed into a series of cadmium salt of concentration successively, after being again stirring for uniformly, applied in ceramic white disk
Upper area is in the same size, uniform one layer of thickness, dries spare；Above-mentioned white disk is divided into two groups, one group of carry out wipe test, separately
One group of carry out stripping quantity experiment；It is fixed that wiping measurement is carried out using graphite oven atomic absorption；Stripping quantity test group is marked according to country
The assay method of quasi- method GB/T 3534-2002 domestic ceramics devices lead, quantity of cadmium release, is carried out using graphite oven atomic absorption
Stripping quantity measures, and records corresponding test data；Finally, using cadmium wiping amount as abscissa, quantity of cadmium release is mapped for ordinate, meter
Calculate the linear relationship deposited between cadmium wiping amount and stripping quantity.
Compared with the prior art, the present invention has the advantages of：The detection of cadmium is limited to 10ng, and entire analysis test process 5~
10min, conventional method and standard method sample treatment need 24 hours, so greatly shortening analysis time, improve working efficiency.
The matched curve regression coefficient of quantity of cadmium release~wiping amount is more than 0.99, illustrates that the present invention speculates stripping quantity using wiping amount is measured
It is feasible.This method have it is easy, quick, easy to operate, disclosure satisfy that the requirement that quantity of cadmium release is quickly analyzed in domestic ceramics.
Description of the drawings
Fig. 1 is quantity of cadmium release and wiping amount linear relationship chart in the present invention.
Specific implementation mode
The present invention is described in further detail below in conjunction with the accompanying drawings.
The present invention is a kind of for measuring quantity of cadmium release detection method in domestic ceramics.When implementing the present invention, need to use
Instrument be：
The UV mini-1240 ultraviolet-uisible spectrophotometers of Japanese Shimadzu Corporation；
The FE20 type pH acidometers of Mettler Toledo Inc.；
800 types of AA and the Atomic Absorption Spectrometer with graphite furnace of Perkinelmer Inc. of the U.S.；
The Synery UV ultrapure water systems of Millipore Corp. of the U.S..
Reagent used in the present invention is：
Cadmium standard solution is selected from State Standard Matter Research Centre, a concentration of 1000mg/L；
Mixed phosphate is selected from Guangzhou Chemical Reagent Factory, purity 99%；
Cadion is selected from lark prestige Science and Technology Ltd.；
Sodium chloride and thiocarbamide are selected from Chinese medicines group chemical reagent Beijing Co., Ltd.
The detection method of the present invention is needed using test paper, wiping agent, color developing agent, colour plate and cadmium standard work color range
Card, wherein
The wiping agent is mixed phosphate salt buffer, a concentration of 1mol/L, pH 9.0；
The color developing agent be by mixed aqueous solution, include according to weight percent：Cadion 0.02%, sodium chloride
0.05%, thiocarbamide 2%, chromogenic reagent solution pH is 9.0；
The cadmium standard works color scale card within the scope of 0~100ng；
When test, the first step cleans domestic ceramics sample to be measured, and naturally dry；
Second step dips wiping agent with test paper, and test paper is folded, and is close to domestic ceramics surface, carry out laterally and
Longitudinal wiping；
Third walks, and the test paper wiped is placed on colour plate, color developing agent in drop, stands, in bright light condition
Under, it compares card with cadmium standard work color range and is compareed, the range of results of cadmium wiping amount in sample is determined with optical colorimetry；
4th step obtains quantity of cadmium release by cadmium wiping amount and stripping quantity linear equation, which is：
Y=0.024x+0.074
Wherein x is cadmium wiping amount, and unit ng, y are quantity of cadmium release, unit mg.
The present invention is specifically described below.
Test paper used in the present invention is dustless quantitative test paper, and the colour plate is white plastic plate.
Wiping agent：Mixed phosphate salt buffer, a concentration of 1mol/L, pH 9.0；Wiping agent matches Preparation Method in the present invention
It is：Dipotassium hydrogen phosphate 5.59g and potassium dihydrogen phosphate 0.41g are weighed, water is diluted to 1000mL, is used in combination 0.1mol/L sodium hydroxides molten
It is 9.0 that liquid, which is adjusted to pH value,.
Color developing agent：Cadion (p-nitrophenyl diazoaminoazobenzene), 0.02% (w/w is formulated in 0.1mol/LNaOH second
Alcoholic solution), sodium chloride 0.05%, the aqueous solution that thiocarbamide 2% is formed.
In order to enable cadmium accurately, fast and efficiently to be detected, selected color developing agent high specificity necessary first, energy
A variety of interfering ions that may be present are enough excluded, it is secondary to have preferable absorptivity in aqueous solution, it is necessary to have significant face
Color change.The chromogenic reaction of cadmium is more complicated with respect to for lead, and 2- (2- pyridines) azo resorcinol complies fully with above-mentioned condition,
But since cadmium belongs to subgroup element in periodic table, there are many elements similar with its character can be dry to its colour developing generation
It disturbs.According to experiment, can be generated in the process color of 2- (2- pyridines) azo resorcinol interference member be known as V, Zn, Co,
Ni, Mn, Cu etc. can shelter the phenanthroline of the interference elements such as Co, to cadmium well since subgroup element character is similar
There is same masking effect.Other screening agents such as EDTA etc. also has same problem.And thiocarbamide is less than 2- to the competition performance of Cu
(2- pyridines) azo resorcinol-Cu, causes the interference of Cu that can not similarly remove.So through finally transferring to have selected in alkali
Cadion --- the p-nitrophenyl diazoaminoazobenzene to develop the color under the conditions of property, this is a kind of color developing agent of relative maturity, is had to cadmium
Preferable selectivity.
After the cadion in color developing agent is determined, chromogenic reagent solution pH value is also predefined.The method that the present invention uses is such as
Under：
0.2g cadions are taken first, are dissolved in the ethanol solution of 0.2mol/LNaOH, and constant volume 100mL, are cadion deposit
Liquid.Triton-X100 (nonionic surfactant) aqueous solution of 10% (V/V) is prepared simultaneously.It is added in 50mL volumetric flasks
400 μ L cadmium standard solution, the Triton-X100 aqueous solutions of 100 μ L 10% is added in 5mL cadion storing solutions.Use ultraviolet spectrometry
Photometer carries out wavelength full scan analysis, and scanning range is 300nm~650nm, and the pH value for adjusting solution be respectively 5.0,
6.5,7.0,8.5,9.0,10,11 and 12, the full wavelength scanner under above-mentioned pH value respectively.The result shows that when pH value is more than 8.0
When, cadmium is combined apparent enhancing, cadion absorption curve to occur an acromion at 475nm and be gradually increasing with cadion, together
When main absorption peak reduce, solution colour becomes red from orange.And pH be more than after 11 cadion occur absorption peak at 553nm,
Itself becomes aubergine, so pH when cadion measures cadmium should be greater than 8, while being less than 11, aobvious through testing final optimization pass confirmation
Toner pH value of solution is 9.0.
Then, color developing agent experiment of eliminating interference is also predefined, method is：Since the interference of cadmium is than more serious, different pH
Under value, the case where disturbance ion is combined from XO, is different, can pass through and adjust pH value removal interference.Visual method is first used in this experiment
The interference of 100mg/LCa, Mg under pH8-11 are eliminated, 9 kinds of elements such as reselection Si, B, Cu, Co, Pb, Ba, Ag, Au, Cr carry out
Interference test.Experimentation is as follows：
200 μ L cadion storing solutions are added in 25mL volumetric flasks, the Triton-X100 of 100 μ L 10% is then added
Aqueous solution.Above-mentioned 9 kinds of interfering ions are sequentially added, and make its a concentration of 100mg/L (Co 50mg/L) in the solution, it is fixed
Hold, using absorbance value of the solution at 620nm as blank, maximum absorption band of the recording solution in Cd-XO --- the suction at 475nm
Shading value, and compared with the absorbance value after solution addition 8mg/LCd.The result shows that：Cu, Co, Ag are when pH value is 9.0, energy
It is enough to be combined with XO and absorption peak occur in close positions, interfere the colour developing of Cd.The removal of Ag interference can also use 0.05%
NaCl.After NaCl is added in the solution, the red that solution is shown after addition Ag is taken off, and absorbance value (A-A0) is reduced to 0.053；
In this system, the combination of Cu and thiocarbamide is better than with XO's.When pH is 9.0, there are one the colour developings of Cd is obviously improved, this
When Co light absorption curve also promoted, but visually the solution colour of Co-XO does not have significant change.Final choice pH9.0 is Cd
Colour developing pH.It can ensure that the absorbance of Cd is good under the pH, while remove the interference of Co to a certain extent.
Cadion is with method for determination of amount in the present invention：The cadmium of 200 μ L is added when colour test in 25mL volumetric flasks
Reagent stock liquid adds the 10%Triton-X100 (aqueous solution) of 100 μ L, finally uses the phosphate buffer solution of pH=9.0
Constant volume.In order to optimize chromogenic agent, it is separately added into the cadion storing solution of 100,200,400,600,800 μ L, to 50ng
Cadmium carry out chromogenic reaction.Test result shows：When cadion dosage is 100 and 200 μ L, blank control group background color is very shallow, and 400
When μ L, blank control group background color is slightly deepened, and 50 μ g/L colour developings are apparent.The cadion background color of 600 μ L and 800 μ L become apparent,
Though having reinforcement but unobvious to the colour developing of cadmium.Finally select 400 μ L for final cadmium storing solution dosage.
The test paper wiping direction of the present invention and number are also determining by experiment, and determination method is：Domestic ceramics table
The quantity of cadmium release in face can reach balance in certain time.In order to keep cadmium dissolution abundant as possible, but the time is saved to the maximum extent,
The optimization of wiping method and number is necessary.Wiping agent is dipped with test paper, test paper is then subjected to 4 refoldings, is close to daily
Ceramic surface, first laterally wiping, then make wiping surface reflexed test paper inwardly, and it is close to domestic ceramics surface, it is longitudinal to wipe.Not to six kinds
The sample that the domestic ceramics quantity of cadmium release experiment of same type is positive carries out the wiping of distinct methods and number.Laterally wiping number
Respectively 2,4,6,8,10 and 12 times, longitudinal number that wipes is respectively 2,4,6,8,10 and 12 times.Then test paper is put into glass
In centrifuge tube, 0.5mL ultra-pure waters are added into centrifuge tube, so that the cadmium on wiping test paper is fully dissolved out after ultrasonic 20min.Then,
After rotating speed is 10000 beats/min of high speed centrifugation 5min, inhales the solution in 20 μ L centrifuge tubes using micro-sampling pin and inject graphite-pipe
In, test cadmium content in solution using graphite furnace atomic absorption spectrometry.The experimental results showed that the wiping amount of cadmium and wiping direction
Related with number, horizontal and vertical combination wiping is wiped significantly better than unidirectional, meanwhile, it is also passed as wiping number increases wiping amount
Increase, when horizontal and vertical wiping number more than 8 times after, the wiping amount of cadmium is held essentially constant, and illustrates that quantity of cadmium release reaches flat
Weighing apparatus, so selecting wiping method for horizontal and vertical wiping, each direction wiping is 8 times.
Determine that the linear relationship of quantity of cadmium release and wiping amount in domestic ceramics, method are：Select the white disk of domestic ceramics for
Research object coats a series of simulation pigment of cadmiums containing various concentration in Bai Panshang respectively, carries out wipe test and stripping quantity examination
It tests, and records wiping amount and stripping quantity, inquire into its linear relationship：Pigment is simulated with boric acid, sodium chloride, calcium nitrate and basic carbonate
Magnesium is matrix.The mixing salt of above-mentioned formula stirs evenly after being added in coating, as bottom material, then is mixed into successively a series of dense
The cadmium salt (cadmium nitrate) of degree.After being again stirring for uniformly, coat that size is consistent, and uniform one layer of thickness is dried in the air in ceramic white disk
It is dry spare.
White disk will be tested and be divided into two groups, every group 6, each white disk volume is about 120mL, one group of carry out wipe test, separately
One group of carry out stripping quantity experiment.For wiping method with number according to horizontal and vertical wiping, each direction wiping is 8 times, is then made
It is fixed that wiping measurement is carried out with graphite oven atomic absorption.Stripping quantity test group method GB/T 3534-2002 days according to national standards
With ware lead, the assay method of quantity of cadmium release, stripping quantity measurement is carried out using graphite oven atomic absorption, and record corresponding survey
Try data.With cadmium wiping amount (ng) for abscissa, quantity of cadmium release (mg) is mapped for ordinate, as shown in Figure 1.As seen from Figure 1, cadmium
There are good linear relationship between wiping amount and stripping quantity, linear equation y=0.024x+0.074, related coefficient is
0.9942。
Determine that the making of cadmium standard work color scale card, method are：Serial cadmium concentration is added drop-wise on test paper, is then added
2 drops wipe agent, are placed on colour plate, add color developing agent.Color after being reacted with the cadmium ion of various concentration colour reagent
Variation is photographed to record, and is fabricated to standard work color scale card.
Embodiment one：
It is derived from domestic ceramics-jorum 12 processed, is divided into two groups, every group 6, one group carries out wipe test by inventive method：
Domestic ceramics sample to be measured is cleaned, and naturally dry, after then dipping wiping agent with test paper, dips wiping agent with test paper, so
Test paper is subjected to 4 refoldings afterwards, is close to domestic ceramics surface, first laterally wiping 8 times, then makes wiping surface reflexed test paper inwardly, tightly
Paste domestic ceramics surface, longitudinal wiping 8 times.Test paper is placed on colour plate, the upper 1 drop color developing agent of drop stands 2 minutes, bright
Under bright light condition, compares card with cadmium standard work color range and compareed, cadmium wiping amount in sample is determined with optical colorimetry
Range of results, and quantity of cadmium release is obtained by cadmium wiping amount and stripping quantity linear equation.Another group of GB/T according to national standards
The assay method of 3534-2003 domestic ceramics devices lead, quantity of cadmium release carries out quantity of cadmium release survey using graphite oven atomic absorption
It is fixed, and corresponding quantity of cadmium release is calculated as a result, first group of domestic ceramics sample wiping amount is converted into stripping quantity, average result is
1.2mg/L, second group of average result that standard GB/T/T 3534-2003 are analyzed according to national standards is 1.4mg/L.
Embodiment two：
It takes laboratory to retain domestic ceramics quantity of cadmium release positive -12, dish, is divided into two groups, every group 6, one group by hair
Bright method carries out wipe test：Domestic ceramics sample to be measured is cleaned, and naturally dry, after then dipping wiping agent with test paper,
Wiping agent is dipped with test paper, test paper is then subjected to 4 refoldings, is close to domestic ceramics surface, first laterally wiping 8 times, then makes wiping
It wipes and faces inner reflexed test paper, be close to domestic ceramics surface, longitudinal wiping 8 times.Test paper is placed on colour plate, upper 1 drop of drop is aobvious
Toner stands 2 minutes, under bright light condition, compares card with cadmium standard work color range and is compareed, use optical colorimetry
It determines the range of results of cadmium wiping amount in sample, and quantity of cadmium release is obtained by cadmium wiping amount and stripping quantity linear equation.It is another
The assay method of group domestic ceramics positive GB/T 3534-2003 domestic ceramicses device lead, quantity of cadmium release according to national standards,
Quantity of cadmium release measurement is carried out using graphite oven atomic absorption, and calculates corresponding quantity of cadmium release as a result, first group of domestic ceramics sample
Product wiping amount is converted into stripping quantity, average result 8.6mg/L, second group of standard GB/T/T 3534- according to national standards
The average result of 2003 analyses is 8.4mg/L.
Embodiment three：
It takes laboratory to retain domestic ceramics quantity of cadmium release positive -12, cup, is divided into two groups, every group 6, one group by hair
Bright method carries out wipe test：Domestic ceramics sample to be measured is cleaned, and naturally dry, after then dipping wiping agent with test paper,
Wiping agent is dipped with test paper, test paper is then subjected to 4 refoldings, is close to domestic ceramics surface, first laterally wiping 8 times, then makes wiping
It wipes and faces inner reflexed test paper, be close to domestic ceramics surface, longitudinal wiping 8 times.Test paper is placed on colour plate, upper 1 drop of drop is aobvious
Toner stands 2 minutes, under bright light condition, compares card with cadmium standard work color range and is compareed, use optical colorimetry
It determines the range of results of cadmium wiping amount in sample, and quantity of cadmium release is obtained by cadmium wiping amount and stripping quantity linear equation.It is another
The measurement side of group domestic ceramics positive cup GB/T 3534-2003 domestic ceramicses device lead, quantity of cadmium release according to national standards
Method carries out quantity of cadmium release measurement using graphite oven atomic absorption, and calculates corresponding quantity of cadmium release as a result, first group of domestic ceramics
Sample wiping amount is converted into stripping quantity, average result 4.2mg/L, second group of standard GB/T/T 3534- according to national standards
The average result of 2003 analyses is 4.3mg/L.
In conjunction with concrete application case, illustrate that the analysis result of the invention accuracy is satisfactory.It is analyzed compared to national standard
Method, the invention have many advantages, such as that quick, easy, easy to operate and accuracy is high, disclosure satisfy that quantity of cadmium release in domestic ceramics
Quickly analysis.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (8)
1. a kind of detection method for measuring quantity of cadmium release in domestic ceramics, it is characterised in that：
This method is needed using test paper, wiping agent, color developing agent, colour plate and cadmium standard work color scale card, wherein described
Wiping agent is mixed phosphate salt buffer, a concentration of 1mol/L, pH 9.0；
The color developing agent be by mixed aqueous solution, include according to weight percent：Cadion 0.02%, sodium chloride
0.05%, thiocarbamide 2%, chromogenic reagent solution pH is 9.0；
The cadmium standard works color scale card within the scope of 0~100ng；
When test, the first step cleans domestic ceramics sample to be measured, and naturally dry；
Second step dips wiping agent with test paper, and test paper is folded, and is close to domestic ceramics surface, carries out horizontal and vertical
Wiping；
Third walks, and the test paper wiped is placed on colour plate, color developing agent in drop, stands, under bright light condition, with
Cadmium standard work color range control card is compareed, and the range of results of cadmium wiping amount in sample is determined with optical colorimetry；
4th step obtains quantity of cadmium release by cadmium wiping amount and stripping quantity linear equation, which is：
Y=0.024x+0.074
Wherein x is cadmium wiping amount, and unit ng, y are quantity of cadmium release, unit mg.
2. a kind of detection method for measuring quantity of cadmium release in domestic ceramics according to claim 1, it is characterised in that：
The test paper is dustless quantitative test paper, and the colour plate is white plastic plate.
3. a kind of detection method for measuring quantity of cadmium release in domestic ceramics according to claim 1, it is characterised in that：
The wiping agent preparation method is：According to dipotassium hydrogen phosphate and potassium dihydrogen phosphate according to 5.29：0.41 weight ratio configures water
Solution, a concentration of 1mol/L, it is 9.0 to be used in combination 0.1mol/L sodium hydroxide solutions to be adjusted to pH value.
4. a kind of detection method for measuring quantity of cadmium release in domestic ceramics according to claim 1, it is characterised in that：
Cadion uses p-nitrophenyl diazoaminoazobenzene in the color developing agent, and its to be formulated in 0.1mol/L NaOH ethyl alcohol molten
In liquid.
5. a kind of detection method for measuring quantity of cadmium release in domestic ceramics according to claim 1, it is characterised in that：
In the second step, test paper is first subjected to 4 refoldings before wiping, is close to domestic ceramics surface, first laterally wiping 8 times, then will
The wiping surface of test paper reflexed inwardly is close to domestic ceramics surface, longitudinal wiping 8 times.
6. a kind of detection side for measuring quantity of cadmium release in domestic ceramics according to any one of claim 1-5
Method, it is characterised in that：The chromogenic reagent solution pH is 9.0, and the method for determining chromogenic reagent solution pH is：0.2g cadions are taken,
It is dissolved in the ethanol solution of 0.2mol/LNaOH, and constant volume 100mL, as cadion storing solution；Prepare 10% (V/V's) simultaneously
Triton-X100 aqueous solutions；
5mL cadion storing solutions are added in 50mL volumetric flasks, 400 μ L cadmium standard solution, the Triton- of 100 μ L 10% is added
X100 aqueous solutions carry out wavelength full scan analysis with ultraviolet specrophotometer, and scanning range is 300nm~650nm, and is adjusted molten
The pH value of liquid is respectively 5.0,6.5,7.0,8.5,9.0,10,11 and 12, respectively the full wavelength scanner under above-mentioned pH value；
It is obtained according to scanning result：When pH value is more than 8.0, cadmium is combined apparent enhancing, cadion absorption curve with cadion
Occur an acromion at 475nm and be gradually increasing, while main absorption peak reduces, solution colour becomes red from orange；And pH
There is absorption peak at 553nm in cadion after more than 11, itself becomes aubergine, so pH when cadion measures cadmium should be greater than
8, while being less than 11, final optimization pass confirms that chromogenic reagent solution pH is 9.0.
7. a kind of detection side for measuring quantity of cadmium release in domestic ceramics according to any one of claim 1-5
Method, it is characterised in that：The cadmium wiping amount and the confirmation method of stripping quantity linear equation be：The white disk of domestic ceramics is selected to grind
Study carefully object, coat a series of simulation pigment of cadmiums containing various concentration in Bai Panshang respectively, carries out wipe test and stripping quantity experiment,
And wiping amount and stripping quantity are recorded, then calculate the linear relationship of the two.
8. a kind of detection method for measuring quantity of cadmium release in domestic ceramics according to claim 7, it is characterised in that：
The cadmium wiping amount is with the confirmation method of stripping quantity linear equation, and the simulation pigment is with boric acid, sodium chloride, calcium nitrate
It is matrix with basic magnesium carbonate；It is stirred evenly after above-mentioned mixing salt is added in coating, as bottom material, then is mixed into one successively
The cadmium salt of series concentration after being again stirring for uniformly, is coated that size is consistent, uniform one layer of thickness in ceramic white disk, is dried
It is spare；
Above-mentioned white disk is divided into two groups, one group of carry out wipe test, another group of carry out stripping quantity experiment；It is inhaled using sampling Graphite Furnace Atomic
It is fixed that receipts method carries out wiping measurement；Method GB/T3534-2002 domestic ceramicses device lead, cadmium are molten according to national standards for stripping quantity test group
The assay method of output carries out stripping quantity measurement using graphite oven atomic absorption, and records corresponding test data；Finally, with
Cadmium wiping amount is abscissa, and quantity of cadmium release is mapped for ordinate, calculates the linear relationship deposited between cadmium wiping amount and stripping quantity.
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