AU2019100861A4 - Rapid detection method of lead content in child paint - Google Patents
Rapid detection method of lead content in child paint Download PDFInfo
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- AU2019100861A4 AU2019100861A4 AU2019100861A AU2019100861A AU2019100861A4 AU 2019100861 A4 AU2019100861 A4 AU 2019100861A4 AU 2019100861 A AU2019100861 A AU 2019100861A AU 2019100861 A AU2019100861 A AU 2019100861A AU 2019100861 A4 AU2019100861 A4 AU 2019100861A4
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- ray fluorescence
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- fluorescence spectrometer
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/61—Specific applications or type of materials thin films, coatings
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to a rapid detection method of lead content in child paint, comprising the following steps: preparing a sample according to the material of the sample by an appropriate method, placing the sample in a sample chamber of an X-ray fluorescence spectrometer, and analyzing the sample according to a selected test mode; using the test conditions recommended by an instrument manufacturer, or adjusting light tube voltage to be 40KV or more; using analytical line lead recommended by the X-ray fluorescence spectrometer, sequentially preferably the analytical line L2-M4 (L31), and the analytical line L3-M4,5 (LUl,2); selecting a standard sample or a reference sample that matches a substrate of a tested sample; referring to Appendix A for sample preparation; determining the fluorescence intensity of a lead element in the standard sample according to the measurement condition of the X-ray fluorescence spectrometer; and drawing a working curve according to a standard value given by the standard sample and a fluorescence intensity value measured by the spectrometer. In the determination method of lead content in child paint in the present invention, the preparation of the sample is close to a coating process of the tested child paint; and the sample is digested with strong acid so that a detection result can reflect the total lead content in the tested child paint.
Description
[0001] The present invention belongs to the technical field of detection, and particularly relates to a rapid detection method of lead content in child paint.
BACKGROUD OF THE PRESENT INVENTION [0002] Child paint is a paint or coating used for renovation and decoration of a child room and protection of child products. Lead is a heavy metal element that does not have any physiological function to a human body and is seriously harmful to human health, and especially may cause irreversible damage to organs and systems at growth and development stages of children. However, the lead is widely used in many fields such as transportation, manufacturing industry, industry, printing and cosmetics. With the rapid development of global modem industry and transportation, air, water sources, soil and food in the natural world are polluted by the lead to different degrees, causing that environmental lead pollution has become a prominent problem to be solved urgently. In particular, articles used for the children, such as toys and study articles, have high lead content, which is an important factor that affects growth and development of the children. WHO believes that “the lead has the greatest threat to the children in the environment”, and lead poisoning of the children has become a global public safety issue and has caused worldwide attention.
SUMMARY OF PRESENT INVENTION [0003] The purpose of the present invention is to overcome the defects in the prior art, so as to provide a rapid detection method of lead content in child paint with accurate operation and detection result.
[0004] The present invention adopts the following technical solution to solve the technical problems:
[0005] The present invention has the advantages and positive effects:
[0006] 1) In the determination method of lead content in child paint in the present invention, since a paint coating includes various organic substances, additives and curing agents, lead-free paint coating powder sheets are selected in the test and added
2019100861 05 Aug 2019 into the corresponding lead standard solutions of different contents to form a to-be-determined solution of the working curve, thereby eliminating the interference of the substrate.
[0007] 2) In the determination method of lead content in child paint in the present invention, the sample is digested with concentrated nitric acid, hydrofluoric acid and perchloric acid and converted into a to-be-determined solution of a submitted sample completely dissolve the lead in the paint coating; and the total lead content in the coating is determined by using an inductively coupled plasma (ICP) emission spectrometer, which is convenient in operation and reduces the use of chemical reagents, so that the measurement result is faster and more accurate, and the performance is stable, reliable and practical.
[0008] 3) In the determination method of lead content in child paint in the present invention, the preparation of the sample is close to a coating process of the tested child paint; and the sample is digested with strong acid so that the detection result can reflect the total lead content in the tested child paint.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS [0009] The present invention is further described in detail below through specific embodiments. The following embodiments are merely illustrative and not restrictive, and shall not be intended to limit the protection scope of the present invention. [0010] A rapid detection method of lead content in child paint comprises the following steps:
[0011] (1) preparing a sample according to the material of the sample by an appropriate method, placing the sample in a sample chamber of an X-ray fluorescence spectrometer, and analyzing the sample according to a selected test mode;
[0012] (2) enabling the size of the homogeneous sample with a smooth material surface (such as homogeneous polymer material, metal material or coating material, and other material) to satisfy the requirements of the X-ray fluorescence spectrometer;
[0013] (3) transferring a liquid sample of a certain volume into a liquid-special plastic cup since the X-ray fluorescence spectrometer has specific requirements for the liquid sample; supporting the bottom of the plastic cup by a polyester film with a thickness of 6 pm; covering the plastic cup with a plastic cover with a hole; and
2019100861 05 Aug 2019 enabling the addition amount of the sample to be a thickness of 2 cm to 3 cm in the plastic cup to ensure that the sample is infinitely thick for X-rays;
[0014] (4) using the polymer material, the metal material and the coating material which have the same uniform physical property for direct determination of by X-ray fluorescence spectrometer; cutting the sample into a size of Φ10 mm to Φ40 mm by a cutter and placing the sample into a sample cup of the fluorescence spectrometer if the sample is too large and does not satisfy the sample test requirements of the spectrometer; requiring the surface to be smooth; and marking the sample;
[0015] (5) since a heterogeneous sample generally cannot be directly tested, freezing the sample by liquid nitrogen, pulverizing the sample into particles smaller than 1.0 mm by a pulverizer and uniformly mixing; making a representative sample under a certain pressure by a tableting machine into a tablet sample; and marking the sample;
[0016] (6) using the test conditions recommended by an instrument manufacturer, or adjusting light tube voltage to be 40KV or more; using analytical line lead recommended by the X-ray fluorescence spectrometer, sequentially preferably the analytical line L2-M4 (Σβί), and the analytical line L3-M4,5 (La 1,2);
[0017] (7) selecting a standard sample or a reference sample that matches a substrate of a tested sample; referring to Appendix A for sample preparation; determining the fluorescence intensity of a lead element in the standard sample according to the measurement condition of the X-ray fluorescence spectrometer; and drawing a working curve according to a standard value given by the standard sample and a fluorescence intensity value measured by the spectrometer;
[0018] (8) placing the prepared sample into the sample chamber; performing X-ray analysis on the sample according to the selected test mode; and performing at least two tests on each sample; and [0019] (9) conducting result analysis.
[0020] 1. Result calculation. The spectral line intensity of the lead element measured by the sample is used to calculate the content of the lead element in the sample according to the selected determination mode.
[0021] The value is rounded, and is accurate to two decimal places; and the value is rounded according to GB/T 8170.
[0022] 2 Precision: Repeatability (r) [0023] In the same laboratory, the same equipment is used by the same operator,
2019100861 05 Aug 2019 and the relative deviation of two test results obtained by testing the same tested object independently according to the same test method within a short time is not more than 10%.
[0024] 3 Reproducibility (R) [0025] In different laboratories, different equipment is used by different operators, and the relative deviation of two independent test results obtained by testing the same tested object independently according to the same test method is not more than 20%. [0026] Embodiment [0027] The present embodiment is used for preparing a reference sample for the test of the X-ray fluorescence spectrometer, and is used for value verification of the test result of the X-ray fluorescence spectrometer.
[0028] instruments: ICP mass spectrometer (mass resolution is better than 0.8 ±0.1 amu), high-pressure microwave digestion instrument and thickness gauge.
[0029] Reagents: nitric acid, lead white (79%), zinc oxide, raw linseed oil, cooked linseed oil, mineral spirit, concentrated nitric acid and ultrapure water.
[0030] Material: natural wood board (90mmx 120mm), asbestos cement board (90mmx 120mm) and glass board (90mmx 120mm).
[0031] Sample Preparation and Processing [0032] 1. The material is prepared as follows: the lead white (79%), the zinc oxide, the raw linseed oil, the cooked linseed oil and the mineral spirit are mixed according to a specific proportion, and thoroughly stirred by a ball mill for dispersion preparation of an experimental paint analog. Refer to the following Table 1 for sample ingredients and formulations.
Table 1 Reference Sample Ingredients and Formulations
| Comp onent | Lead White | Zinc Oxide | Raw Linseed Oil | Cooked Linseed Oil | Mineral Spirit | Theoretical Concentration * (%) |
| 1# | 0g | 600 g | 70 g | 70 g | 70 g | 0 |
| 2# | 13 g | 587 g | 70 g | 70 g | 70 g | 1.02 |
[0033] *This refers to the mass percentage concentration of lead in the paint analog prepared in a laboratory.
[0034] 2. Gradient Preparation and Processing of Reference Sample [0035] The first group (1#) is a blank paint sample without the addition of lead
2019100861 05 Aug 2019 white, and the second group (2#) is a paint sample with the addition of lead white. The theoretical concentration is 1% (10 g/kg). The concentrations of 200 mg/kg (3#), 120 mg/kg (4#), 90 mg/kg(5#), 60 mg/kg(6#), 40 mg/kg(7#) and 30 mg/kg(8#) are obtained by different ratios of 1# and 2#.
[0036] 3. Paint Film Thickness of Paint Film Reference Sample [0037] The concentration gradient prepared for the gradient preparation and processing preparation of the reference sample in step 2 is applied to A.2.3 material on not less than 5 points selected. The paint film thickness of the standard sample is measured according to the national standard: GB/T 13452.2. A micrometer is used to measure the paint film thickness, i.e., a difference between the thickness of a substrate paint film and the thickness of the substrate. A non-destructive method can be used: measurement is performed before and after the paint is coated, i.e., the thickness of the substrate is measured at first; and after the paint is coated, the substrate is naturally aired or dried at a temperature not more than 60°C, and the total thickness of the same measurement region is measured. The paint film thickness can be calculated from the difference between two readings. Five points are selected for each substrate for test, and the paint film thickness is required as follows:
[0038] The paint film thickness of a glass product in a child room is greater than or equal to 20±2 pm;
[0039] The paint film thickness of a wood product in the child room is greater than or equal to 45±3 pm; and [0040] The paint film thickness of interior wall paint in the child room is greater than or equal to 80±9 pm.
[0041] 4. Determination of Fead Concentration in Reference Sample [0042] (1) Sample Preparation [0043] The coating material on the sample is scraped off by using a blade or other proper scraping tools at room temperature. It should be noted that the substrate material of the sample shall not be scraped. The scraped coating material is ground at room temperature for later use.
[0044] (2) Sample Digestion [0045] The sample is pre-processed with reference to the method in EPA3051 A, and the sample is weighed at about 0.1 g, accurate to 0.1 mg, and placed in a microwave digestion tank, and 10 mF of concentrated nitric acid is respectively added. The digestion tank is closed and conducts digestion according to the
2019100861 05 Aug 2019 following temperature program: the temperature is raised to (175 ± 5)°C in approximately 5.5 min, maintained for 10 min and then decreased. After the digestion tank is cooled to room temperature, the digestion tank is opened; the digestion solution is transferred to a volumetric flask of 25 mL; a microwave digestion inner tank and a microwave digestion inner cover are washed with a small amount of nitric acid for three times; and the washing liquid is incorporated into the volumetric flask and diluted with water to a scale. If the digestion solution is not clear or precipitated, the solution shall be filtered and the residual solid material is rinsed with 5 mL of nitric acid for three times. All the obtained solutions are combined and transferred into a volumetric flask of 50 mL, and diluted with water to a constant volume of 50 mL, and the filtrate is analyzed by an instrument as soon as possible. A blank test is conducted for the sample.
[0046] (3) Determination of Total Lead Content of Sample [0047] In this test, the ICP-MS method is used to determine the blank lead content of the sample solution and the reagent. The result is accurate to two decimal places, and the value is rounded according to GB/T 8170.
Claims (2)
- (1) preparing a sample according to the material of the sample by an appropriate method, placing the sample in a sample chamber of an X-ray fluorescence spectrometer, and analyzing the sample according to a selected test mode;(2) enabling the size of the homogeneous sample with a smooth material surface to satisfy the requirements of the X-ray fluorescence spectrometer;(3) transferring a liquid sample of a certain volume into a liquid-special plastic cup since the X-ray fluorescence spectrometer has specific requirements for the liquid sample;(4) using polymer material, metal material and coating material which have the same uniform physical property for direct determination of by X-ray fluorescence spectrometer; cutting the sample into a size of Φ10 mm to Φ40 mm by a cutter and placing the sample into a sample cup of the fluorescence spectrometer if the sample is too large and does not satisfy the sample test requirements of the spectrometer; requiring the surface to be smooth; and marking the sample;(5) since a heterogeneous sample generally cannot be directly tested, freezing the sample by liquid nitrogen, pulverizing the sample into particles smaller than 1.0 mm by a pulverizer and uniformly mixing; making a representative sample under a certain pressure by a tableting machine into a tablet sample; and marking the sample;(6) using the test conditions recommended by an instrument manufacturer, or adjusting light tube voltage to be 40KV or more; using analytical line lead recommended by the X-ray fluorescence spectrometer, sequentially preferably the analytical line L2-M4 (L β 1), and the analytical line L3-M4,5 (Lal,2);(7) selecting a standard sample or a reference sample that matches a substrate of a tested sample; referring to Appendix A for sample preparation; determining the fluorescence intensity of a lead element in the standard sample according to the measurement condition of the X-ray fluorescence spectrometer; and drawing a working curve according to a standard value given by the standard sample and a fluorescence intensity value measured by the spectrometer; and (8) placing the prepared sample into the sample chamber; performing X-ray analysis on the sample according to the selected test mode; and performing at least two tests on each2019100861 05 Aug 2019 sample.1. A rapid detection method of lead content in child paint, comprising the following steps:
- 2. The rapid detection method of lead content in child paint according to claim 1, wherein the bottom of the plastic cup is supported by a polyester film with a thickness of 6 pm; covering the plastic cup with a plastic cover with a hole; and enabling the addition amount of the sample to be a thickness of 2 cm to 3 cm in the plastic cup to ensure that the sample is infinitely thick for X-rays.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2019100861A AU2019100861A4 (en) | 2019-08-05 | 2019-08-05 | Rapid detection method of lead content in child paint |
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| AU2019100861A AU2019100861A4 (en) | 2019-08-05 | 2019-08-05 | Rapid detection method of lead content in child paint |
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| AU2019100861A4 true AU2019100861A4 (en) | 2019-09-12 |
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| AU2019100861A Ceased AU2019100861A4 (en) | 2019-08-05 | 2019-08-05 | Rapid detection method of lead content in child paint |
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Cited By (1)
| 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 |
-
2019
- 2019-08-05 AU AU2019100861A patent/AU2019100861A4/en not_active Ceased
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 |
| 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 |
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| MK22 | Patent ceased section 143a(d), or expired - non payment of renewal fee or expiry |