CN110988098B - Method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution - Google Patents
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Abstract
The invention belongs to the field of determination of heavy metals in water-based adhesives for cigarettes, and particularly relates to a method for determining various heavy metals in water-based adhesives for cigarettes after direct dilution. Taking a multi-element mixed standard solution containing arsenic, lead, cadmium, chromium and nickel elements, diluting with 5% nitric acid to a constant volume to obtain the multi-element mixed standard solution of arsenic, lead, cadmium, chromium and nickel with different concentrations; preparing a sample blank solution according to the steps; selecting Ge, in and Bi elements as internal standards, and drawing a standard curve; calculating the concentration of each element from the standard line; and (4) according to the weight of the weighed water-based adhesive and the calculated concentration of each element. The method is simple to operate, avoids the risks of pollution, tube explosion corrosion and the like caused by complex sample pretreatment, shortens the sample pretreatment time, improves the sample analysis speed, and is particularly suitable for detecting heavy metals in batch water-based adhesive samples.
Description
Technical Field
The invention belongs to the field of determination of heavy metals in water-based adhesives for cigarettes, and particularly relates to a method for determining various heavy metals in water-based adhesives for cigarettes after direct dilution.
Background
The water-based adhesive for cigarettes is a high molecular polymer, is an adhesive prepared from a film-forming material which can be dispersed or dissolved in water, is also called a water-soluble adhesive, is a common adhesive in cigarette production, and is also an important component of a filter tip. Because the filter tip is directly contacted with the oral cavity during suction, heavy metals (such as arsenic, lead, cadmium, chromium and nickel) contained in the water-based adhesive can easily enter the human body. Heavy metal elements can react with protein and enzyme to reduce the physiological activity of the tobacco leaves, interfere normal metabolism and have great influence on the health of smokers. Hitherto, in addition to determination of heavy metal elements in water-based adhesives by using a strong acid solution combined with a microwave digestion method (the [ subject name ] ICP-MS method for determination of chromium, nickel, cadmium and lead in water-based adhesives [ author ] Wang Wenyuan, flame blue, xia Jianjun, etc., technical research and development center of limited liability company of red-shipping red river tobacco (group) [ publication name ] northhu agricultural science, 2013,52 (24): 6148-6233, entitled method for measuring heavy metals in water-based adhesive for cigarettes by inductively coupled plasma mass spectrometry (author) Xiong Wen, shu Yunbo, zhang Junsong, etc., (entitled method for measuring heavy metal elements such as arsenic, lead, cadmium, chromium, nickel, etc. in water-based adhesive for cigarettes by inductively coupled plasma mass spectrometry (unpublished) in Anhui agriculture, 2011,17 (8) 40, 88, entitled method for measuring chromium, nickel, arsenic, selenium, cadmium, mercury and lead in materials for cigarettes by inductively coupled plasma mass spectrometry (industry standard) YC/T316-2014), and a method for measuring heavy metal elements such as arsenic, lead, cadmium, chromium, nickel, etc. in water-based adhesive after direct dilution is not reported.
At present, the pretreatment of a water-based adhesive sample is carried out only after a strong acid is added and the sample is treated by microwave digestion, and the pretreatment method of the sample has the defects of long time consumption, tube explosion, corrosion, large solvent consumption, easy pollution and high detection cost. Therefore, the development of a method for determining the content of the heavy metal in the water-based adhesive after direct dilution without digestion is of great significance.
Disclosure of Invention
The invention provides a method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution, aiming at solving various problems in the pretreatment process during the existing water-based adhesive measurement.
The invention is realized by the following technical scheme: a method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution comprises the following steps:
(1) preparation of standard working solutions: taking a multi-element mixed standard solution containing arsenic, lead, cadmium, chromium and nickel elements, diluting the multi-element mixed standard solution with 5% nitric acid to a constant volume to obtain the multi-element mixed standard solution of arsenic, lead, cadmium, chromium and nickel with different concentrations, wherein the concentrations are 0.2 mu g/L, 0.5 mu g/L, 1.0 mu g/L, 2.0 mu g/L, 5.0 mu g/L, 10.0 mu g/L, 20.0 mu g/L, 40.0 mu g/L, 60.0 mu g/L and 100.0 mu g/L;
(2) preparation of test sample solution: weighing 0.3g of water-based glue of the neutral line glue, adding ultrapure water to dilute to 50mL, uniformly mixing, and standing for later use;
(3) sample blank solution: preparing a sample blank solution according to the method in the step (2);
(4) and (3) determination: adding a mixed internal standard solution containing Ge, in and Bi elements on line, respectively measuring 5% nitric acid In a standard blank solution and a standard working solution by using an inductively coupled plasma mass spectrometer, and drawing a standard curve by taking the ratio of the mass-to-charge ratio intensity of the element to be measured to the mass-to-charge ratio intensity of the corresponding internal standard element as a vertical coordinate and the concentration as a horizontal coordinate; measuring the sample blank solution and the sample solution to be tested by using an inductively coupled plasma mass spectrometer, measuring in parallel for three times, bringing the three times into a standard curve, and calculating the concentration of each element from the standard curve;
(5) and (4) analyzing results: calculating the contents of arsenic, lead, cadmium, chromium and nickel in the water-based glue of the neutral line glue according to the weight of the weighed water-based glue of the neutral line glue and the calculated concentration of each element:
in the formula: c is the element concentration in the sample solution, mu g/L; c 0 The concentration of elements in a sample blank solution is shown as mu g/L; v is the volume of the test sample solution, mL; m is the mass g of the water-based glue of the midline glue.
In the present invention, the water-based glue of the center line glue type is referred to as center line glue. Similarly, the water-based glue of the non-midline glue is worth other water-based glue except the midline glue, and mainly comprises lap glue, packaging glue and joint glue.
The invention further provides a method for measuring various heavy metals in the water-based adhesive for cigarettes after direct dilution, which is characterized by comprising the following steps:
(1) preparation of standard working solutions: taking a multi-element mixed standard solution containing arsenic, lead, cadmium, chromium and nickel elements, diluting the multi-element mixed standard solution with 5% nitric acid to a constant volume to obtain the multi-element mixed standard solution of arsenic, lead, cadmium, chromium and nickel with different concentrations, wherein the concentrations are 0.2 mu g/L, 0.5 mu g/L, 1.0 mu g/L, 2.0 mu g/L, 5.0 mu g/L, 10.0 mu g/L, 20.0 mu g/L, 40.0 mu g/L, 60.0 mu g/L and 100.0 mu g/L;
(2) preparation of test sample solution: weighing 0.3g of water-based glue of non-midline glue, adding 5% SDS solution to dilute to 50mL, mixing uniformly, and standing for later use;
(3) sample blank solution: preparing a sample blank solution according to the method in the step (2);
(4) and (3) determination: adding a mixed internal standard solution containing Ge, in and Bi elements on line, respectively measuring 5% nitric acid In a standard blank solution and a standard working solution by using an inductively coupled plasma mass spectrometer, wherein the ratio of the mass-to-charge ratio intensity of the element to be measured to the mass-to-charge ratio intensity of the corresponding internal standard element is a vertical coordinate, the concentration is a horizontal coordinate, and drawing a standard curve; measuring the sample blank solution and the sample solution to be tested by using an inductively coupled plasma mass spectrometer, measuring in parallel for three times, bringing the three times into a standard curve, and calculating the concentration of each element from the standard curve;
(5) and (4) analyzing results: calculating the contents of arsenic, lead, cadmium, chromium and nickel in the water-based glue of the non-midline glue according to the weight of the weighed water-based glue of the non-midline glue and the calculated concentration of each element:
in the formula: c is the element concentration in the sample solution, mu g/L; c 0 The element concentration in the sample blank solution is shown as mu g/L; v is the volume of the test sample solution, mL; m is the mass g of the water-based glue of the non-midline glue.
In the method for measuring the water-based glue of the midline glue and the water-based glue of the non-midline glue, the volume of the sample solution to be tested is equal to the volume of the sample blank solution.
As a further improvement of the technical scheme of the present invention, the operating conditions of the inductively coupled plasma mass spectrometer are as follows: radio frequency power 1550w; plasma gas 15L/min; the flow rate of the carrier gas is 1.0L/min; the flow rate of the auxiliary gas is 1.0L/min; the sample introduction rate is 0.1rps; and obtaining full quantitative analysis of the mode.
According to the method for determining multiple heavy metals in the water-based adhesive for cigarettes, a water-based adhesive sample with a certain mass is directly dissolved in 50mL of ultrapure water or 5% of SDS (sodium dodecyl sulfate) solution, and a diluent is directly taken for determination.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a standard curve of chromium (Cr).
Fig. 2 is a standard curve of nickel (Ni).
FIG. 3 is a standard curve of arsenic (As).
FIG. 4 is a standard curve for cadmium (Cd).
Fig. 5 is a standard curve of lead (Pb).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example (b): determination of contents of various heavy metals in 4 water-based adhesive samples
1. Actual sample measurement results
Test samples (samples 1-4, where sample 1 is a midline adhesive, sample 2 is a lap adhesive, sample 3 is a nozzle adhesive, and sample 4 is a packaging adhesive);
10 mu g/mL and 100 mL/bottle of multielement heavy metal mixed standard solution, agilent company;
100 mu g/mL of internal standard solution containing Sc, ge, in and Bi elements, 50 mL/bottle, agilent company.
2. Measurement work
(1) Online internal standard solution: a certain volume of internal standard solution (Agilent company, the concentration of which is 100 mu g/mL internal standard solution) containing Ge, in and Bi elements is diluted to 0.5 mu g/mL by using 5 percent nitric acid solution (5 wt percent) as an online internal standard.
(2) Preparation of standard working solutions: taking a certain volume of multi-element standard solution (Agilent, 10 mu g/mL standard solution), adopting 5% nitric acid solution (5 wt%), and preparing working solution according to the concentration shown in Table 1
TABLE 1 contents of As, pb, cd, cr and Ni elements in the standard solution (. Mu.g/L)
(3) Accurately weighing 0.3g (accurate to 0.0001 g) of sample in a plastic bottle of 1-100 mL, adding ultrapure water for dissolving, diluting and fixing the volume to 50mL, carrying out ultrasonic extraction for 30min at normal temperature by using 100KHz power, standing for a period of time, and taking supernatant into a sample tube.
(4) Weighing 0.3g (accurate to 0.0001 g) of sample (2, 3, 4) into a 100mL plastic bottle, adding 5% SDS solution to dissolve, diluting to 50mL, performing ultrasonic extraction at normal temperature with 100KHz power for 30min, standing for a period of time, and taking supernatant to be put into a sample tube.
(5) Blank sample: four 100mL plastic bottles are used, no sample is added, only 50mL of ultrapure water or 5% SDS solution is added, ultrasonic extraction is carried out for 30min at normal temperature by using 100KHz power, then the upper layer solution is taken out to a sample tube after standing for a period of time, and two types of blank solutions are obtained to be tested.
(6) Working conditions of inductively coupled plasma mass spectrometer
Adjusting the inductively coupled plasma mass spectrometer to a state suitable for working by using tuning liquid, and then setting working parameters of the inductively coupled plasma mass spectrometer: radio frequency power 1550w; plasma gas 15L/min; the flow rate of the carrier gas is 1.0L/min; the flow rate of the auxiliary gas is 1.0L/min; the sample introduction rate is 0.1rps; obtaining a full quantitative analysis of a mode; the number of repetitions was 3. And (3) carrying out sample injection measurement by an automatic sample injection system with the model of ASX 500. The elements to be measured, the internal standard elements and the integration time are shown in table 2.
TABLE 2 Mass number of elements to be measured, internal standard element and integration time
| Element name | Measuring isotopes | Internal standard element | Integration time |
| Chromium (III) | 53 | Germanium (Ge-72) | 0.3s |
| Nickel (II) | 60 | Germanium (Ge-72) | 0.3s |
| Arsenic (As) | 75 | Germanium (Ge-72) | 1.0s |
| Cadmium (Cd) | 111 | Indium (In-115) | 0.5s |
| Lead (II) | 208 | Bismuth (Bi-209) | 0.3s |
(7) Drawing a standard curve and comparing the test results of the test samples: carrying out quantitative analysis on heavy metal elements of chromium, nickel, arsenic, cadmium and lead by an internal standard method, namely carrying out linear regression analysis on the concentrations of the heavy metal elements of chromium, nickel, arsenic, cadmium and lead according to the ratio of the response values of the elements of chromium, nickel, arsenic, cadmium and lead to the response values of the corresponding internal standard elements to obtain a standard curve (the result is shown in attached figures 1-5). Substituting the ratio of the response value of each element in the sample solution measured under the same condition to the response value of the corresponding internal standard element into the standard curve to obtain the mass concentration of the element to be measured in the sample solution, and calculating the content of the element to be measured in the original sample by using the dilution factor, wherein the results of measuring the test samples (1-4) by using the direct dilution method in the embodiment are shown in table 3. Meanwhile, an industry standard (YC/T316-2014) method is adopted: the results of the microwave digestion of the samples to determine the test samples (1-4) are detailed in Table 3. According to the results, the heavy metal content in the water-based adhesive for cigarettes can be accurately measured by the two methods. Compared with a standard method, the sample pretreatment of the embodiment (direct dilution method) is simpler and quicker, the risks of tube explosion corrosion and the like possibly caused by microwave digestion are avoided, the detection period of the sample is shortened, the working efficiency of detection personnel is improved, and the method is more suitable for detection of the water-based adhesive samples in batches.
TABLE 3 determination of the heavy Metal content in the test samples (1-4) (unit. Mu.g/kg)
Note: column "a" data was determined using direct dilution of the sample; the "b" column data was determined by microwave digestion of the samples using the industry standard (YC/T316-2014) method.
(8) Linear equation, detection limit and lower limit of quantitation:
the blank solution was subjected to 10 measurements, and the standard deviation was calculated, with 3-fold standard deviation as the detection limit and 10-fold standard deviation as the lower limit of quantitation, and the results are shown in table 4. As can be seen by combining the figure and the table 4, the correlation coefficient of the regression equation of each element reaches more than 0.999, the lower limit of the quantification is not more than 50 mug/kg, and the quantification requirement is met.
TABLE 4 detection limit, quantitative limit, recovery rate and relative standard deviation of each element of Cr, ni, as, cd and Pb
(9) Recovery and standard deviation:
three levels of standard solutions (2. Mu.g/L, 5. Mu.g/L, 10. Mu.g/L) were added to the samples (1-4) using the standard addition method, and the measurements were performed using the treatment methods and measurement conditions given in the examples, and the method recoveries and standard deviations were calculated, and the results are shown in Table 4. As can be seen from Table 4, the relative standard deviation determined was not greater than 5.76, which is a good reproducibility; the recovery rates of the five elements of chromium, nickel, arsenic, cadmium and lead are all in the range of 88.40% -108.85%, which shows that the method can accurately determine the five elements of chromium, nickel, arsenic, cadmium and lead in the water-based adhesive sample and is suitable for quantitative analysis of heavy metal elements in batch water-based adhesive samples.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (2)
1. A method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution is characterized by comprising the following steps:
(1) preparation of standard working solutions: taking the multi-element mixed standard solution containing arsenic, lead, cadmium, chromium and nickel elements, diluting with 5% nitric acid to a constant volume to obtain the multi-element mixed standard solution of arsenic, lead, cadmium, chromium and nickel with different concentrations, wherein the concentrations are 0.2 mu g/L, 0.5 mu g/L, 1.0 mu g/L, 2.0 mu g/L, 5.0 mu g/L, 10.0 mu g/L, 20.0 mu g/L, 40.0 mu g/L, 60.0 mu g/L and 100.0 mu g/L;
(2) preparation of test sample solution: weighing 0.3g of water-based glue of the neutral line glue, adding ultrapure water to dilute to 50mL, uniformly mixing, and standing for later use;
(3) sample blank solution: preparing a sample blank solution according to the method in the step (2);
(4) and (3) determination: adding a mixed internal standard solution containing Ge, in and Bi elements on line, respectively measuring 5% nitric acid In a standard blank solution and a standard working solution by using an inductively coupled plasma mass spectrometer, wherein the ratio of the mass-to-charge ratio intensity of the element to be measured to the mass-to-charge ratio intensity of the corresponding internal standard element is a vertical coordinate, the concentration is a horizontal coordinate, and drawing a standard curve; measuring the sample blank solution and the sample solution to be tested by using an inductively coupled plasma mass spectrometer, measuring in parallel for three times, bringing the three times into a standard curve, and calculating the concentration of each element from the standard curve; the working conditions of the inductively coupled plasma mass spectrometer are as follows: radio frequency power 1550w; plasma gas 15L/min; the flow rate of the carrier gas is 1.0L/min; the flow rate of the auxiliary gas is 1.0L/min; the sample introduction rate is 0.1rps; obtaining a full quantitative analysis of a mode;
(5) and (4) analyzing results: according to the weight of the weighed water-based glue of the neutral line glue and the calculated concentration of each element, calculating to obtain the content of arsenic, lead, cadmium, chromium and nickel in the water-based glue of the neutral line glue:
in the formula: c is the element concentration in the sample solution, mu g/L; c 0 The concentration of elements in a sample blank solution is shown as mu g/L; v is the volume of the test sample solution, mL; m is the mass g of the water-based glue of the midline glue.
2. A method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution is characterized by comprising the following steps:
(1) preparation of standard working solutions: taking a multi-element mixed standard solution containing arsenic, lead, cadmium, chromium and nickel elements, diluting the multi-element mixed standard solution with 5% nitric acid to a constant volume to obtain the multi-element mixed standard solution of arsenic, lead, cadmium, chromium and nickel with different concentrations, wherein the concentrations are 0.2 mu g/L, 0.5 mu g/L, 1.0 mu g/L, 2.0 mu g/L, 5.0 mu g/L, 10.0 mu g/L, 20.0 mu g/L, 40.0 mu g/L, 60.0 mu g/L and 100.0 mu g/L;
(2) preparation of test sample solution: weighing 0.3g of water-based glue of non-midline glue, adding 5% SDS solution to dilute to 50mL, mixing uniformly, and standing for later use;
(3) sample blank solution: preparing a sample blank solution according to the method in the step (2);
(4) and (3) determination: adding a mixed internal standard solution containing Ge, in and Bi elements on line, respectively measuring 5% nitric acid In a standard blank solution and a standard working solution by using an inductively coupled plasma mass spectrometer, wherein the ratio of the mass-to-charge ratio intensity of the element to be measured to the mass-to-charge ratio intensity of the corresponding internal standard element is a vertical coordinate, the concentration is a horizontal coordinate, and drawing a standard curve; measuring the sample blank solution and the sample solution to be tested by using an inductively coupled plasma mass spectrometer, measuring in parallel for three times, bringing the three times into a standard curve, and calculating the concentration of each element from the standard curve; the working conditions of the inductively coupled plasma mass spectrometer are as follows: radio frequency power 1550w; plasma gas 15L/min; the flow rate of the carrier gas is 1.0L/min; the flow rate of the auxiliary gas is 1.0L/min; the sample introduction rate is 0.1rps; acquisition mode full quantitative analysis
(5) And (4) analyzing results: calculating the contents of arsenic, lead, cadmium, chromium and nickel in the water-based glue of the non-midline glue according to the weight of the weighed water-based glue of the non-midline glue and the calculated concentration of each element:
in the formula: c is the element concentration in the sample solution, mu g/L; c 0 The concentration of elements in a sample blank solution is shown as mu g/L; v is the volume of the test sample solution, mL; m is the mass g of the water-based glue of the non-midline glue.
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