CN106752530A - A kind of preparation method of lead-based paint standard sample - Google Patents
A kind of preparation method of lead-based paint standard sample Download PDFInfo
- Publication number
- CN106752530A CN106752530A CN201611233669.0A CN201611233669A CN106752530A CN 106752530 A CN106752530 A CN 106752530A CN 201611233669 A CN201611233669 A CN 201611233669A CN 106752530 A CN106752530 A CN 106752530A
- Authority
- CN
- China
- Prior art keywords
- sample
- lead
- based paint
- preparation
- high speed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of preparation method of lead-based paint standard sample, crylic acid resin varnish coat is painted as matrix using general toy material, by adding target heavy metal element, disperse at a high speed, grinding is mixed, obtain lead-based paint standard sample, the Pb testing results relative deviation of the sample is no more than 15%, sample inhomogeneities standard deviation is not more than 0.3 σ, the uniformity and stability of sample meet the requirement of proficiency testing sample, blank of the China currently without such proficiency testing sample is filled up, improve the detection level for participating in proficiency testing laboratory.
Description
Technical field：
The present invention relates to a kind of preparation method of lead-based paint standard sample.
Background technology：
Standard sample is not only the basis of chemical analysis transmission of quantity value, and is also that detection and analysis process carries out quality management
Instrument, standard sample is respectively provided with important effect at the aspect such as instrument calibration, method validation and evaluation, quality control, and it can
To ensure the validity and comparativity of measurement result.US Consumer Product Safety Commission CPSC 16CFR1303 and U.S.'s consumer goods
The regulations of improvements in security bill CPSIA 101 have the limitation requirement of total lead to the material in juvenile product and toy, in order to ensure
China's export meets the lead tolerance requirement of the above to the product in the U.S., it is necessary to the content of experimental material.To ensure assay
Accuracy, it is therefore necessary to the related juvenile product test stone sample of research.The leaded highest risk in numerous toy materials
Material is painting layer, however, the toy inspection field still national standard sample in kind without leaded coating matrix at present.Play
Containing total lead heavy metal analysis it is most important toy safety in tool coating, is also most classical detection project, therefore, prepare leaded heavy
Metal coating sample has filled up the blank of China's lead-based paint standard sample, for the accuracy of laboratory detection result provide according to
According to, it is ensured that the quality safety of juvenile product and toy.
The content of the invention：
It is an object of the invention to provide a kind of preparation method of lead-based paint standard sample.
The present invention is achieved by the following technical programs：
A kind of preparation method of lead-based paint standard sample, the method is comprised the following steps：
1) prepares stock white：In mass ratio it is 3：1 weighs titanium dioxide and alkyd resin, at high speed dispersor (ZQ4113)
Upper dispersion 2H makes that material is well mixed to obtain stock white；
2) prepares leaded wet paint：By step 1) stock white that obtains is with crylic acid resin varnish, organic pigment content
It is organic pigment alcoholic solution, aluminum paste, copper powder, the lead naphthenate class drier that lead content is 24wt%, the dilution of 3-4wt%
After agent mixing, leaded wet paint is uniformly obtained with color is dispersed to by slow-to-fast in 500-2500 revs/min of high speed dispersor；Its
In middle mixture, by mass percentage, stock white is 25%, and crylic acid resin varnish accounts for 72.6-73.2wt%, You Jiyan
Material alcoholic solution is 0.3%, and aluminum paste accounts for 1.0%, and copper powder accounts for 0.5%, and lead naphthenate class drier is 0.0125%-
0.625%, balance of diluent；
3) sprayings：ABS (acrylonitrile/butadiene/styrene copolymer) blackboard eraser is tried clean with ethyl acetate, by step
2) after the leaded wet paint high speed dispersor that obtains disperses 30 minutes, appropriate diluent is added, is stirred while by paint
Load in spray gun, spray immediately, each plate is sprayed three times, and every block of plate there are 0.5g dry paints；
4) dries in the air plate：The place that the plate that will have been sprayed is placed on ventilation dries and to obtain within 1 week Pb concentration ranges for 30-1500mg/kg
Target product, is stored in temperature less than in 35 DEG C, the sample cabinet of constant temperature and humidity of the humidity less than 60%.
Step 1) alkyd resin is preferably short oil-ity alcohol acid resin.
Base material of the present invention selects the general ebonite paint crylic acid resin varnish of toy, adds universal white slurry and organic pigment
Alcoholic solution adjusts painting color；Using the conventional lead drier of paint as the material for introducing lead element；Choose toy normal
With plastic cement base material A BS (acrylonitrile/butadiene/styrene copolymer) plates as spraying sheet material；In addition, in paint introduce aluminium,
The interference elements such as copper, to increase the difficulty of lead element test.
Beneficial effects of the present invention are as follows：
The present invention paints crylic acid resin varnish coat as matrix using general toy material, by adding target
Heavy metal element, at a high speed dispersion, grinding are mixed, and obtain lead-based paint standard sample, and the Pb concentration ranges of the sample are 30-
1500mg/kg, Pb testing result relative deviation are no more than 15%, and sample inhomogeneities standard deviation is not more than 0.3 σ, sample
Uniformity and stability meet the requirement of proficiency testing sample, have filled up sky of the China currently without such proficiency testing sample
In vain, the detection level for participating in proficiency testing laboratory is improved.
Brief description of the drawings：
Fig. 1 is the structural representation of standard sample of the invention.
Specific embodiment：
Further illustrated the following is to of the invention, rather than limitation of the present invention.
Embodiment 1：It is the orange lead-based paint standard samples of the 4.8kg (numbering of 75mg/kg to prepare a concentration containing Pb
H1501)
Comprise the following steps：
1. stock white is prepared：In mass ratio it is 3：1 weighs titanium dioxide and short oil-ity alcohol acid resin, in high speed dispersor
(ZQ4113) material is well mixed to obtain stock white to disperse 2H to make on；
2. leaded wet paint is prepared：The stock white that step 1 is obtained is with crylic acid resin varnish, organic pigment content
The organic pigment alcoholic solution of 3-4%wt, aluminum paste, copper powder, lead content are lead naphthenate class drier, the diluent of 24wt%
After mixing, disperse about 2H that leaded wet paint is uniformly obtained to color by slow-to-fast with 500-2500 revs/min of high speed dispersor；
Wherein in mixture, by mass percentage, stock white is 25%, and crylic acid resin varnish accounts for 73.17wt%, You Jiyan
Material alcoholic solution is 0.3%, and aluminum paste accounts for 1.0%, and copper powder accounts for 0.5%, and lead naphthenate class drier is 0.0313%, balance of
Diluent；
3. spray：ABS (acrylonitrile/butadiene/styrene copolymer) blackboard eraser is tried clean with ethyl acetate, it is standby；Will
After leaded wet paint high speed dispersor that step 2 is obtained disperses 30 minutes, appropriate diluent is added, stirred while by oil
Paint loads in spray gun, sprays immediately, and each plate is sprayed three times, and every block of plate has 0.5g dry paints.
4. dry in the air plate：The place drying that the plate that will have been sprayed is placed on ventilation obtains target product in 1 week, is by spray plate order after collection
Every piece of plate numbering, is stored in sample cabinet temperature less than 35 DEG C, stand-by in the sample cabinet of constant temperature and humidity of the humidity less than 60%.
Base material of the present invention selects the general ebonite paint crylic acid resin varnish of toy, adds universal white slurry and organic pigment
Alcoholic solution adjusts painting color；Using the conventional lead class drier of paint as the material for introducing lead element；Choose toy
Conventional plastic cement base material A BS (acrylonitrile/butadiene/styrene copolymer) plates are used as spraying sheet material；In addition, being introduced in paint
The interference elements such as aluminium, copper, to increase the difficulty of lead element test.
Embodiment 2：The uniformity test of sample
By CNAS-GL03:2006《Proficiency testing sample homogeneity and estimation of stability guide》, using single-factor variance point
The uniformity of its sample room is checked in analysis.
The orange lead-based paint standard sample (H1501) obtained to embodiment 1 randomly selects 10, respectively numbering 1 to 10,
By the standards of GB/T 22788 about the total Determination of Pb of toy painting layer corresponding clause disposal ability checking article, using electricity
Sense coupled plasma spectrometer determines the content of total lead in sample.Each sample weighs two samples and is put down under the conditions of repeatability
Row is determined twice, and Counting statistics amount F variance test values the results are shown in Table 1.
Proficiency testing article uniformity testing result (mg/kg) of table 1
Table look-up F0.05 (9,10)=3.02, and statistic F values are respectively less than critical value, as a result show：Sample room is poor without conspicuousness
It is different, show that the proficiency testing article of preparation is uniform.
(σ is the proficiency testing projected capacity evaluation criterion of IQTC14C01 for calculating inhomogeneities standard deviation and 0.3 σ respectively
Deviation：Sane standard deviation s*), inhomogeneities standard deviation S s≤0.3 σ further demonstrates this proficiency testing and in the works can
Power checking article is uniform.
Embodiment 3：Sample tissue ability verification is verified
Embodiment 2 is detected that qualified sample assigns to 152 laboratories by uniformity, is entered according to unified experimental arrangement
The Concentration Testing of the total lead content of row, testing result and statistics table are as shown in table 2.
The testing result and statistics table of the total lead content of table 2
Note：# represents problematic result；§ meaning results with thumb down.
Testing result relative deviation is no more than 15%.
Embodiment 4, sample stability is detected
By ISO13528:2005 Appendix B《Sample homogeneity and stability test》Carry out, commented using unstability deviation method
Estimate the stability of proficiency testing article.
After the recovery of proficiency testing result, 3 bottles of samples are randomly selected, tested according to uniformity test condition.Every bottle
Sample weigh two samples under the conditions of repeatability parallel determination twice, the average value of computation and measurement, using unstability deviation
Method whether there is significant difference between comparing two groups of average values of different time test result.
The stability test assay (mg/kg) of table 3
Result shows：The overall average of this proficiency testing proficiency testing article uniformity testing and stability test in the works
Value difference valueThe characteristic quantity for this proficiency testing is may infer that, the sample of preparation is stable.
In sum, the uniformity and stability of sample of the invention meet the requirement of proficiency testing sample.
Claims (2)
1. a kind of preparation method of lead-based paint standard sample, it is characterised in that the method is comprised the following steps：
1) in mass ratio it is 3：1 weighs titanium dioxide and alkyd resin, disperse 2H to make material well mixed on high speed dispersor
To stock white；
2) by step 1) stock white that obtains is the organic pigment of 3-4wt% with crylic acid resin varnish, organic pigment content
Alcoholic solution, aluminum paste, copper powder, lead content be 24wt% lead naphthenate classes drier, diluent mixing after, use high speed dispersor
Color is dispersed to by slow-to-fast in 500-2500 revs/min and uniformly obtains leaded wet paint；Wherein in mixture, by quality percentage
Than meter, stock white 25%, crylic acid resin varnish accounts for 72.6-73.2wt%, and organic pigment alcoholic solution is 0.3%, aluminium silver
Slurry accounts for 1.0%, and copper powder accounts for 0.5%, and lead naphthenate class drier is 0.0125%-0.625%, balance of diluent；
3) ABS blackboard erasers being tried clean with ethyl acetate, by step 2) the leaded wet paint high speed dispersor that obtains disperses 30 points
Zhong Hou, adds diluent, stirs while by paint loading spray gun, spraying immediately, each plate is sprayed three times, and every block of plate has
0.5g dry paints；
4) plate that will have been sprayed is placed on the local of ventilation and dries the target product for obtaining that Pb concentration ranges are 30-1500mg/kg for 1 week,
Temperature is stored in less than in 35 DEG C, the sample cabinet of constant temperature and humidity of the humidity less than 60%.
2. the preparation method of lead-based paint standard sample according to claim 1, it is characterised in that step 1) alkyd
Resin is short oil-ity alcohol acid resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233669.0A CN106752530A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method of lead-based paint standard sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233669.0A CN106752530A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method of lead-based paint standard sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106752530A true CN106752530A (en) | 2017-05-31 |
Family
ID=58922615
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611233669.0A Pending CN106752530A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method of lead-based paint standard sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106752530A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323282A (en) * | 2020-04-10 | 2020-06-23 | 广州海关技术中心 | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field |
| CN113776902A (en) * | 2021-08-16 | 2021-12-10 | 拱北海关技术中心 | Preparation method of reference standard substance for detecting impurities in aluminum pigment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031537A (en) * | 2014-06-13 | 2014-09-10 | 安徽华业建工集团有限公司 | Coating and preparation method thereof |
| CN105136532A (en) * | 2015-07-24 | 2015-12-09 | 东莞市诚标检测科技有限公司 | Lead-containing paint coating standard substance and preparation method thereof |
-
2016
- 2016-12-28 CN CN201611233669.0A patent/CN106752530A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031537A (en) * | 2014-06-13 | 2014-09-10 | 安徽华业建工集团有限公司 | Coating and preparation method thereof |
| CN105136532A (en) * | 2015-07-24 | 2015-12-09 | 东莞市诚标检测科技有限公司 | Lead-containing paint coating standard substance and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323282A (en) * | 2020-04-10 | 2020-06-23 | 广州海关技术中心 | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field |
| CN111323282B (en) * | 2020-04-10 | 2022-09-06 | 广州海关技术中心 | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field |
| CN113776902A (en) * | 2021-08-16 | 2021-12-10 | 拱北海关技术中心 | Preparation method of reference standard substance for detecting impurities in aluminum pigment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105092571A (en) | Method for quickly detecting application performance of titanium dioxide of oil paint systems | |
| CN104497826B (en) | A kind of woodenware PU color inhibition matte varnish being sprayed on white finish paint | |
| CN109443864B (en) | Sample preparation method for detecting weather resistance of titanium dioxide | |
| CN103396702B (en) | Preparation method of heavy metal-containing crayon standard sample for laboratory capability verification | |
| CN104761692A (en) | Modification method for introducing carbon-carbon double bond to surface of nanometer silicon dioxide | |
| CN106752530A (en) | A kind of preparation method of lead-based paint standard sample | |
| CN102269719A (en) | X-fluorescence film-pressing method for measuring content of components in ferric oxide powder | |
| CN104535642A (en) | A method of measuring a plurality of heavy metals in an organic pigment by a microwave digestion-inductively coupled plasma mass spectrometry | |
| CN103760302A (en) | Method for testing mixing uniformity of dry powder | |
| CN109704348A (en) | A kind of dedicated flatting silica of water paint and preparation method thereof | |
| CN112986060A (en) | Method for detecting dispersibility of titanium dioxide in oil paint | |
| CN111323282A (en) | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field | |
| CN102433039B (en) | Aqueous high-molecular dispersant, preparation method thereof, and purpose thereof | |
| CN110006796A (en) | A kind of test method of plastics titanium dioxide partial size | |
| CN108827993A (en) | Realize quickly measurement high performance magnetic material BMS-12 in lanthanum, calcium, cobalt each element content method | |
| CN110954394A (en) | Method for measuring content of nickel, copper, aluminum, chromium and molybdenum in recarburizing agent by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) | |
| CN108593692A (en) | EU REACH Legislation height pays close attention to the leather standard sample and preparation method of substance X fluorescence spectrum standard measure screening | |
| CN103308357A (en) | Lead-containing paint coating standard substance and preparation method thereof | |
| Quevauviller | Certified reference materials for the quality control of inorganic analyses of manufactured products (glass, polymers, paint coatings) | |
| CN105086578A (en) | Method and product for adjusting color difference of stone-like paint and application | |
| CN104390839B (en) | Cream kind cosmetic standard material containing heavy metal Hg element and preparation method thereof | |
| CN105136532B (en) | A kind of leaded painting layer standard substance and preparation method | |
| WO2021098128A1 (en) | Mixed sample quantitative test method and apparatus for chemical test items of consumer product | |
| AU2019100861A4 (en) | Rapid detection method of lead content in child paint | |
| CN107462567A (en) | A kind of method for determining lithium content in zirconium and zircaloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |
|
| RJ01 | Rejection of invention patent application after publication |