CN111220692A - Method for detecting content of heavy metal in food contact material - Google Patents

Method for detecting content of heavy metal in food contact material Download PDF

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Publication number
CN111220692A
CN111220692A CN202010056948.4A CN202010056948A CN111220692A CN 111220692 A CN111220692 A CN 111220692A CN 202010056948 A CN202010056948 A CN 202010056948A CN 111220692 A CN111220692 A CN 111220692A
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filter residue
solution
detected
acid solution
powder
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王富强
王会芳
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Sgs Cstc Standards Technical Services Tianjin Co ltd
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Sgs Cstc Standards Technical Services Tianjin Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4077Concentrating samples by other techniques involving separation of suspended solids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4077Concentrating samples by other techniques involving separation of suspended solids
    • G01N2001/4088Concentrating samples by other techniques involving separation of suspended solids filtration

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a method for detecting the content of heavy metal in a food contact material, which comprises the following steps of taking a paper sample to be detected, and crushing the paper sample to obtain powder to be detected; step two, sequentially adding an acid solution and an oxidant into the powder to be detected, and uniformly mixing to obtain a mixture; step three, performing ultrasonic extraction and centrifugal treatment on the mixture, and filtering by using a microporous filter membrane to obtain filtrate A and filter residue A; step four, repeating the processes from the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, washing the filter residue B with distilled water, combining a cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating, concentrating and cooling the mixed solution, filtering the concentrated solution through a microporous filter membrane, and then diluting to a constant volume to obtain a solution to be detected; and step five, measuring the content of the heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry. The method provided by the invention can be used for extracting heavy metal elements in paper products more thoroughly, and the result of measuring the content of heavy metal in the paper products is closer to the real content of the heavy metal elements, so that the method has a reference value.

Description

Method for detecting content of heavy metal in food contact material
Technical Field
The invention relates to the technical field of detection. More specifically, the invention relates to a method for detecting the content of heavy metals in food contact materials.
Background
Heavy metals generally refer to metal elements with a density greater than 5, such as lead, chromium, cadmium, mercury, arsenic, etc., which can cause harm to human health. The paper food contact material is one of the traditional food contact materials, is widely applied in daily life, and has great influence on the health of human bodies on the quality. However, plant fibers for paper making can absorb free heavy metals in the nature in the growing process, a lot of chemical reagents are always used in the paper making process, further pollution is caused, illegal enterprises can use waste paper to process the waste paper into new paper, toxic heavy metals can be contained in ink fillers in the waste paper, and the content of the heavy metals in food packaging paper exceeds the standard, so that the heavy metal content detection of paper food contact materials is particularly important.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a method for detecting the content of the heavy metal in the food contact material, wherein the detection result is closer to the true value of the content of the heavy metal in the paper product, and the result is more reliable and has higher reference value.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for detecting the content of heavy metals in a food contact material, comprising the steps of:
step one, taking a paper sample to be detected, fully crushing the paper sample to be detected into powder of 50-100 microns, and sieving the powder with a 150-mesh sieve to obtain powder to be detected;
adding an acid solution 9-15 times the weight of the powder to be detected, stirring for 20-30 minutes while adding, standing for 25-35 minutes, then adding an oxidant 7-13 times the weight of the powder to be detected, stirring for 20-30 minutes while adding, uniformly mixing, and standing for 25-35 minutes to obtain a mixture;
step three, placing the mixture into an ultrasonic generator for ultrasonic extraction for 40-50 minutes, then centrifuging the mixture, and filtering with a microporous filter membrane with the pore diameter of 40-50 microns to obtain filtrate A and filter residue A;
step four, repeating the processes from the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, fully washing the filter residue B with distilled water, then combining the cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating and concentrating the mixed solution to 1/10-1/6 of the original volume, cooling to room temperature, filtering the concentrated solution through a microporous filter membrane with the aperture of 0.25-0.30 mu m, and then diluting to a constant volume to obtain a solution to be measured;
and step five, measuring the content of heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
Preferably, in the method for detecting the content of heavy metals in food contact materials, the acid solution is a mixed acid solution of any two of a nitric acid solution with a mass fraction of 45%, a hydrochloric acid solution with a mass fraction of 45% and an acetic acid solution with a mass fraction of 50%;
the method for adding the mixed acid solution comprises the following steps: adding one acid solution while stirring for 10-20 minutes, uniformly mixing, then adding the other acid solution, uniformly stirring for 10 minutes at a constant speed, and uniformly mixing.
Preferably, in the method for detecting the content of heavy metals in food contact materials, the weight ratio of the acid solution added first to the acid solution added later in the mixed acid solution is 2: 1.
Preferably, in the method for detecting the content of heavy metal in food contact material, the oxidizing agent is hydrogen peroxide solution.
Preferably, in the method for detecting the content of the heavy metal in the food contact material, in the second step, the weight of the acid solution is 12 times that of the powder to be detected, and the weight of the oxidant is 10 times that of the powder to be detected.
Preferably, in the method for detecting the content of heavy metal in food contact material, the heavy metal element includes at least one of lead, cadmium, chromium, mercury and arsenic.
The invention at least comprises the following beneficial effects: the method provided by the invention can be used for extracting the heavy metal elements in the paper product more thoroughly, and the result of measuring the content of the heavy metal in the paper product is closer to the real content, more accurate and has a reference value.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail with reference to specific examples, so that those skilled in the art can implement the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials, if not otherwise specified, are commercially available; the specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Step one, taking a paper food packaging box sample to be detected, fully crushing the paper food packaging box sample into 100 mu m powder, and sieving the powder with a 150-mesh sieve to obtain the powder to be detected;
adding a nitric acid solution with the mass fraction of 45% 10 times of the weight of the powder to be detected into the powder to be detected, stirring for 20 minutes while adding, uniformly mixing, then adding a hydrochloric acid solution with the mass fraction of 45% 5 times of the weight of the powder to be detected, uniformly stirring for 10 minutes at a constant speed, uniformly mixing, standing for 35 minutes, then adding a hydrogen peroxide solution with the weight of 13 times of the powder to be detected, stirring for 20 minutes while adding, uniformly mixing, and standing for 35 minutes to obtain a mixture;
step three, placing the mixture into an ultrasonic generator for ultrasonic extraction for 50 minutes, then centrifuging the mixture, and filtering the mixture by using a microporous filter membrane with the pore diameter of 50 microns to obtain filtrate A and filter residue A;
step four, repeating the processes of the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, fully washing the filter residue B with distilled water, then combining the cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating and concentrating the mixed solution to 1/10 with the original volume, cooling to room temperature, filtering the concentrated solution through a microporous filter membrane with the aperture of 0.30 mu m, and then diluting to a constant volume to obtain a solution to be measured;
and step five, measuring the content of heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
Example 2
Step one, taking a paper food packaging box sample to be detected, fully crushing the paper food packaging box sample into 80 mu m powder, and sieving the powder with a 150-mesh sieve to obtain the powder to be detected;
adding 8 times of hydrochloric acid solution with the mass fraction of 45% into the powder to be detected, stirring for 15 minutes while adding, uniformly mixing, then adding 50% acetic acid solution with the mass fraction of 4 times of the powder to be detected, uniformly stirring for 10 minutes at a constant speed, uniformly mixing, standing for 30 minutes, then adding hydrogen peroxide solution with the weight of 10 times of the powder to be detected, stirring for 25 minutes while adding, uniformly mixing, and standing for 30 minutes to obtain a mixture;
step three, putting the mixture into an ultrasonic generator for ultrasonic extraction for 45 minutes, then centrifuging the mixture, and filtering the mixture by using a microporous filter membrane with the pore diameter of 45 mu m to obtain filtrate A and filter residue A;
step four, repeating the processes of the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, fully washing the filter residue B with distilled water, then combining the cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating and concentrating the mixed solution to 1/8 with the original volume, cooling to room temperature, filtering the concentrated solution through a microporous filter membrane with the aperture of 0.25 mu m, and then diluting to a constant volume to obtain a solution to be measured;
and step five, measuring the content of heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
Example 3
Step one, taking a paper food packaging box sample to be detected, fully crushing the paper food packaging box sample into 50 mu m powder, and sieving the powder with a 150-mesh sieve to obtain the powder to be detected;
adding a nitric acid solution with a mass fraction of 45% 6 times of the weight of the powder to be detected into the powder to be detected, stirring for 10 minutes while adding, uniformly mixing, then adding an acetic acid solution with a mass fraction of 50% 3 times of the weight of the powder to be detected, uniformly stirring for 10 minutes at a constant speed, uniformly mixing, standing for 25 minutes, then adding a hydrogen peroxide solution with a weight fraction of 7 times of the weight of the powder to be detected, stirring for 30 minutes while adding, uniformly mixing, and standing for 35 minutes to obtain a mixture;
step three, placing the mixture into an ultrasonic generator for ultrasonic extraction for 40 minutes, then centrifuging the mixture, and filtering the mixture by using a microporous filter membrane with the pore diameter of 40 mu m to obtain filtrate A and filter residue A;
step four, repeating the processes of the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, fully washing the filter residue B with distilled water, then combining the cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating and concentrating the mixed solution to 1/6 with the original volume, cooling to room temperature, filtering the concentrated solution through a microporous filter membrane with the aperture of 0.25 mu m, and then diluting to a constant volume to obtain a solution to be measured;
and step five, measuring the content of heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
Comparative example 1
Taking the same paper food packaging box sample to be detected, preparing a solution to be detected by adopting a common method (such as a wet digestion method), and then measuring the content of heavy metal in the solution to be detected by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
Comparative example 2
And taking the same paper food packaging box sample to be measured, and measuring the content of heavy metal in the paper sample to be measured by adopting an atomic absorption spectrometry.
The results of the measurements of the examples are reported in the following statistical table, in which the content of each heavy metal is measured three times and averaged, in units of measure: (mg/kg).
Lead (II) Cadmium (Cd) Chromium (III) Mercury Arsenic (As)
Example 1 4.52 0.093 4.06 1.25 1.95
Example 2 4.72 0.092 4.09 1.35 2.05
Example 3 4.72 0.088 3.98 1.33 1.98
Comparative example 1 3.72 0.076 3.88 0.61 1.36
Comparative example 2 3.82 0.078 3.95 0.52 1.21
As seen from the data in the table, compared with the detection methods adopted in the comparative example 1 and the comparative example 2, the heavy metal content in the food packaging paper material measured by the method is higher, the paper sample to be measured is firstly crushed into powder, so that the paper sample to be measured is favorably in full contact with the acid solution and the oxidant, the reaction area is increased, and the reaction is more thorough; ultrasonic extraction is adopted to promote the soluble metal elements to be more fully dissolved, centrifugal operation enables metal ions and non-metal substances to be fully separated in a layered mode, and then the metal ions and the non-metal substances can be more effectively separated through filtration of a microporous filter membrane, so that the metal ions can be more purely extracted; the paper sample to be detected reacts with the acid solution and the oxidant for many times, and is subjected to ultrasonic treatment, centrifugation and filtration, so that the metal elements in the paper sample to be detected can be dissolved more fully; the concentration operation further improves the concentration of metal ions, and the detection sensitivity can be increased; the method can fully show that the heavy metal elements, particularly lead, mercury and arsenic, in the paper sample can be extracted more thoroughly, the detection result is closer to the true value of the heavy metal content in the paper sample to be detected, the result is more reliable, and the method has reference value.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.

Claims (6)

1. The method for detecting the content of the heavy metal in the food contact material is characterized by comprising the following steps of:
step one, taking a paper sample to be detected, fully crushing the paper sample to be detected into powder of 50-100 microns, and sieving the powder with a 150-mesh sieve to obtain powder to be detected;
adding an acid solution 9-15 times the weight of the powder to be detected, stirring for 20-30 minutes while adding, standing for 25-35 minutes, then adding an oxidant 7-13 times the weight of the powder to be detected, stirring for 20-30 minutes while adding, uniformly mixing, and standing for 25-35 minutes to obtain a mixture;
step three, placing the mixture into an ultrasonic generator for ultrasonic extraction for 40-50 minutes, then centrifuging the mixture, and filtering with a microporous filter membrane with the pore diameter of 40-50 microns to obtain filtrate A and filter residue A;
step four, repeating the processes from the step two to the step three on the filter residue A to obtain a filter residue B and a filter residue B, fully washing the filter residue B with distilled water, then combining the cleaning solution with the filter residue A and the filter residue B to obtain a mixed solution, evaporating and concentrating the mixed solution to 1/10-1/6 of the original volume, cooling to room temperature, filtering the concentrated solution through a microporous filter membrane with the aperture of 0.25-0.30 mu m, and then diluting to a constant volume to obtain a solution to be measured;
and step five, measuring the content of heavy metal in the solution to be measured by adopting an inductively coupled plasma mass spectrometry (ICP-MS).
2. The method for detecting the content of heavy metals in a food contact material according to claim 1, wherein the acid solution is a mixed acid solution of any two of a nitric acid solution with a mass fraction of 45%, a hydrochloric acid solution with a mass fraction of 45%, and an acetic acid solution with a mass fraction of 50%;
the method for adding the mixed acid solution comprises the following steps: adding one acid solution while stirring for 10-20 minutes, uniformly mixing, then adding the other acid solution, uniformly stirring for 10 minutes at a constant speed, and uniformly mixing.
3. The method for detecting the content of heavy metals in food contact materials according to claim 2, wherein the weight ratio of the acid solution added first to the acid solution added later in the mixed acid solution is 2: 1.
4. The method of claim 1, wherein the oxidizing agent is an aqueous hydrogen peroxide solution.
5. The method for detecting the content of heavy metals in food contact materials according to claim 1, wherein in the second step, the weight of the acid solution is 12 times that of the powder to be detected, and the weight of the oxidant is 10 times that of the powder to be detected.
6. The method according to claim 1, wherein the heavy metal element comprises at least one of lead, cadmium, chromium, mercury, and arsenic.
CN202010056948.4A 2020-01-16 2020-01-16 Method for detecting content of heavy metal in food contact material Pending CN111220692A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114414509A (en) * 2021-12-30 2022-04-29 通标标准技术服务(天津)有限公司 Method for detecting heavy metal chromium in food
CN114674910A (en) * 2022-03-17 2022-06-28 惠州市农业科学研究所(广东省(惠州)区域性农业试验中心) Method for detecting heavy metals in soil

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CN108677015A (en) * 2018-05-14 2018-10-19 陆春景 The method for recycling rare precious metal from waste and old lambda sensor
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CN102539597A (en) * 2011-05-24 2012-07-04 四川省中医药科学院 Method for quickly identifying notopterygium incisum seed and notopterygium franchetii seed
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Publication number Priority date Publication date Assignee Title
CN114414509A (en) * 2021-12-30 2022-04-29 通标标准技术服务(天津)有限公司 Method for detecting heavy metal chromium in food
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