阅读说明：本技术 一种塑胶玩具中重金属含量的初步筛查方法 (Preliminary screening method for heavy metal content in plastic toy ) 是由 杨晓兵 高欣 赵萌迪 张冀飞 于 2020-06-11 设计创作，主要内容包括：本发明提供了一种塑胶玩具中重金属含量的初步筛查方法,涉及有害元素检测技术领域。本发明所述初步筛查方法包括以下步骤：将塑胶玩具拆分为基体样品和涂层样品；利用X射线荧光光谱法对所述基体样品和涂层样品分别进行检测,得到基体和涂层中各重金属元素含量；当重金属元素含量＜GB 6675.4中规定的重金属迁移量限量,则判定塑胶玩具中相应重金属元素含量合格；当重金属元素含量≥GB 6675.4中规定的重金属迁移量限量,则判定塑胶玩具中相应重金属元素含量超标。本发明提供的方法简单,检测用时少；同时,所得检测结果可靠、准确性高,能够用于塑胶玩具中重金属含量的初步筛查。(The invention provides a primary screening method for heavy metal content in a plastic toy, and relates to the technical field of harmful element detection. The preliminary screening method comprises the following steps: splitting the plastic toy into a substrate sample and a coating sample; respectively detecting the substrate sample and the coating sample by using an X-ray fluorescence spectrometry method to obtain the contents of each heavy metal element in the substrate and the coating; when the content of the heavy metal elements is less than the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy is qualified; and when the content of the heavy metal elements is larger than or equal to the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy exceeds the standard. The method provided by the invention is simple, and the detection time is short; meanwhile, the obtained detection result is reliable and high in accuracy, and can be used for preliminary screening of heavy metal content in the plastic toy.)

1. A primary screening method for heavy metal content in a plastic toy is characterized by comprising the following steps:

splitting the plastic toy into a substrate sample and a coating sample;

respectively detecting the substrate sample and the coating sample by using an X-ray fluorescence spectrometry method to obtain the contents of each heavy metal element in the substrate and the coating;

when the content of the heavy metal elements is less than the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy is qualified;

and when the content of the heavy metal elements is larger than or equal to the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy exceeds the standard.

2. The preliminary screening method of claim 1, wherein when the content of heavy metal elements is greater than or equal to the limit of heavy metal migration amount specified in GB6675.4, the method further comprises measuring the heavy metal migration amount by using inductively coupled plasma spectrometry.

3. The primary screening method of claim 1, wherein the coating sample is detected in powder form; the method for obtaining the powdery coating sample comprises the following steps: scraping the coating from the matrix, and grinding into powder to obtain a coating sample; the powder was able to pass through a sieve having a pore size of 0.5 mm.

4. The primary screening method of claim 1 or 3, wherein the matrix sample and the coating sample are to completely cover a detection spot of an X-ray fluorometer; the thickness of the substrate sample and the coating sample is independently more than or equal to 5 mm.

5. The primary screening method of claim 1, wherein the mode of detection is non-metallic.

Technical Field

The invention relates to the technical field of harmful element detection, in particular to a primary screening method of a plastic toy.

Background

China is a large producing and consuming country of children toys and also a main export country of international toy products. Chemical substances in the toy are easy to migrate into children through saliva, sweat and gastric juice, so that the health of the children is endangered, and GB6675.1-2014 and regulations and standards of countries all over the world impose mandatory requirements on harmful heavy metal elements in the toy. And the children toy has the characteristics of various types, complex materials and the like. The existing test methods mainly comprise an inductively coupled plasma spectroscopy (ICP-OES) method, an inductively coupled plasma mass spectrometry (ICP-MS) method and the like, but have the problems of complex operation, long detection period, high requirements on experimenters and the like.

Therefore, a rapid and accurate preliminary screening method for heavy metal content in toys is urgently needed to be established.

Disclosure of Invention

The invention provides a preliminary screening method for heavy metal content in a plastic toy. The screening method obtains the total content of the heavy metal elements in the plastic toy through an X-ray fluorescence method, and judges the condition that the content of the heavy metal elements in the plastic toy exceeds the standard through comparing the total content of the heavy metal elements with the limit value of heavy metal migration quantity specified in GB 6675.4.

The invention provides a primary screening method for heavy metal content in a plastic toy, which comprises the following steps:

splitting the plastic toy into a substrate sample and a coating sample;

respectively detecting the substrate sample and the coating sample by using an X-ray fluorescence spectrometry method to obtain the contents of each heavy metal element in the substrate and the coating;

when the content of the heavy metal elements is less than the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy is qualified;

and when the content of the heavy metal elements is larger than or equal to the limit of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy exceeds the standard.

Preferably, when the content of the heavy metal elements is not less than the limit of the heavy metal migration amount specified in GB6675.4, the method further comprises the step of measuring the heavy metal migration amount by using an inductively coupled plasma spectrometry.

Preferably, the coating sample is tested in powder form; the method for obtaining the powdery coating sample comprises the following steps: scraping the coating from the matrix, and grinding into powder to obtain a coating sample; the powder was able to pass through a sieve having a pore size of 0.5 mm.

Preferably, the matrix sample and the coating sample completely cover the detection light spot of the X-ray fluorescence instrument; the thickness of the substrate sample and the coating sample is more than or equal to 5 mm.

Preferably, the mode of detection is non-metallic.

The invention provides a primary screening method for heavy metal content in a plastic toy, which comprises the following steps: splitting the plastic toy into a substrate sample and a coating sample; respectively detecting the substrate sample and the coating sample by using an X-ray fluorescence spectrometry method to obtain the contents of each heavy metal element in the substrate and the coating; when the content of the heavy metal elements is less than the limit value of the heavy metal migration amount specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy is qualified; and when the content of the heavy metal elements is larger than or equal to the limit value of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy exceeds the standard. The method provided by the invention is simple, and the detection time is short; meanwhile, the obtained detection result is reliable and high in accuracy, and can be used for preliminary screening of heavy metal content in the toy.

Drawings

FIG. 1 is a photograph of a plastic automobile toy tested in accordance with example 1.

Detailed Description

The invention provides a primary screening method for heavy metal content in a plastic toy, which comprises the following steps:

splitting the plastic toy into a substrate sample and a coating sample;

respectively detecting the substrate sample and the coating sample by using an X-ray fluorescence spectrometry method to obtain the contents of each heavy metal element in the substrate and the coating;

when the content of the heavy metal elements is less than the limit value of the heavy metal migration amount specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy is qualified;

and when the content of the heavy metal elements is larger than or equal to the limit value of the heavy metal migration quantity specified in GB6675.4, judging that the content of the corresponding heavy metal elements in the plastic toy exceeds the standard.

The plastic toy is split into a substrate sample and a coating sample.

In the present invention, the coating sample is preferably detected in the form of a powder; the method for obtaining a sample of a powdery coating preferably comprises the following steps: scraping the coating from the matrix, and grinding into powder to obtain a coating sample; the powder is preferably capable of passing through a sieve having a pore size of 0.5 mm.

In the present invention, when the coating layer is applied to the base body of the plastic toy, it is preferable that the coating layer is removed to obtain a coating layer sample. In the present invention, the substrate sample is preferably cut and/or polished before the detection to obtain a substrate sample with a suitable size and a flat surface for the detection.

In the invention, the thicknesses of the coating sample and the matrix sample are preferably not less than 5mm independently, and further are preferably 5-6 mm independently; when the thickness of the matrix sample is less than 5mm, the matrix samples are preferably stacked to meet the thickness requirement. In the present invention, the coating sample is preferably placed in a sample cup for detection; in order to make the thickness of the coating sample meet the test requirements, the powdered coating sample is preferably stacked in a sample cup to a thickness that meets the test requirements. In the invention, the sample cup is a special consumable for the X-ray fluorescence spectrometer, the bottom is a special thin film, the periphery is plastic and does not contain a target object, and the peripheral plastic cannot be detected during detection, so that the detection result is not influenced.

After a substrate sample and a coating sample are obtained, the substrate sample and the coating sample are respectively detected by using an X-ray fluorescence spectrometry method, so that the contents of each heavy metal element in the substrate and the coating are obtained.

In the invention, the coating sample and the substrate sample preferably completely cover the detection light spot of an X fluorescence spectrometer when being detected; the diameter of the detection spot is preferably < 3 mm.

In the present invention, the mode of detection is preferably non-metallic.

In the invention, when the content of the heavy metal element is less than the limit value of the heavy metal migration amount specified in GB6675.4, the content of the heavy metal element in the plastic toy is judged to be qualified; and when the content of the heavy metal elements is larger than or equal to the limit value of the heavy metal migration quantity specified in GB6675.4, judging that the content of the heavy metal elements in the plastic toy exceeds the standard.

When the content of the heavy metal elements is more than or equal to the limit value of the heavy metal migration amount specified in GB6675.4, the method preferably further comprises the step of measuring the heavy metal migration amount by using an inductively coupled plasma spectrometry.

In the invention, the inductively coupled plasma spectrometry is preferably a detection method in GB6675.4, and specifically comprises the following steps: mixing hydrochloric acid solution with a concentration of 0.07mol/L at 37 +/-2 ℃ corresponding to 50 times the mass of the test sample by using a suitable container; if the mass of the test sample is between 10mg and 100mg, only 5mL of 0.07mol/L hydrochloric acid solution is required to be mixed with the test sample, the pH value is adjusted to be 1-1.5, the mixed solution is continuously oscillated for 1h at the temperature of (37 +/-2) ℃ by using a constant temperature oscillator under the condition of keeping out of the sun, and then the mixed solution is kept stand for 1 h; then filtering, and testing the obtained filtrate on a machine; the test conditions are as follows: the incident power is 1100W; the flow rate of cooling gas Ar is 20.0L/min; the flow of the auxiliary gas Ar is 0.3L/min; the Ar flow of the atomizing gas is 25 psi; the rinsing time was 20s and the residence time was 40 s.

The following will describe the preliminary screening method for heavy metal content in plastic toys provided by the present invention in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.