CN109655448B - Method for measuring urinary lead by inductively coupled plasma atomic emission spectrometry - Google Patents
Method for measuring urinary lead by inductively coupled plasma atomic emission spectrometry Download PDFInfo
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- CN109655448B CN109655448B CN201910011558.2A CN201910011558A CN109655448B CN 109655448 B CN109655448 B CN 109655448B CN 201910011558 A CN201910011558 A CN 201910011558A CN 109655448 B CN109655448 B CN 109655448B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention relates to the technical field of urinary lead detection, in particular to a method for detecting urinary lead by an inductively coupled plasma atomic emission spectrometry, which is used for solving the defects that the pretreatment process is complicated, the lead loss or pollution is easy to cause, and the accuracy of the result is greatly influenced in the prior art, and comprises the following steps: step 1, preparing a standard lead solution: preparing a plurality of portions of fresh morning urine with the same volume, respectively adding the portions of fresh morning urine into a triangular beaker, adding a nitric acid solution, evaporating the nitric acid solution at a low temperature until the volume of the fresh morning urine is 1/4-1/6 times that of the fresh morning urine, adding a perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down the urine, cooling the urine, using a small amount of deionized water to rinse the wall of the beaker, adding a hydrochloric acid solution, and heating and boiling the solution to obtain a solution for preparing a lead standard series matrix. The method for detecting the content of the lead in the urine by the triacid pretreatment inductively coupled plasma emission method has the advantages of high analysis speed, high sensitivity, good precision and the like, can better meet the test requirement of the content of the lead in the urine, and is worthy of popularization.
Description
Technical Field
The invention relates to the technical field of urinary lead detection, in particular to a method for detecting urinary lead by an inductively coupled plasma atomic emission spectrometry.
Background
Lead is one of the earliest metals used by humans. The danger of lead poisoning has long been recognized by humans. In the modern society, scientific technology develops rapidly, the application of lead is wider, and the harm to human health is larger and larger. Industrial lead poisoning always occupies the first place in the middle virus cases of chronic occupational diseases in China, and chronic poisoning caused by lead can damage the hematopoietic system, the nervous system, the kidney and the like of a human body. GB 5009.12 provides five methods for detecting lead content, which are graphite furnace atomic absorption spectrometry, hydride atomic fluorescence spectrometry, flame atomic absorption spectrometry, dithizone colorimetry and single scanning polarography. The five conventional detection methods all need to perform testing after propylene glycol is incinerated or digested to a water phase, and the pretreatment process is complex and complicated, lead loss or pollution is easily caused, and the accuracy of the result is greatly influenced.
The inductively coupled plasma atomic emission spectrometry is the fastest-developing inorganic trace element analysis technology since the 80 th century, is widely applied to the aspects of food, biological samples, water quality analysis and the like, and has the characteristics of low detection limit, wide linear range, accuracy, rapidness, multi-element simultaneous analysis and the like. Through a large number of experiments, the method for detecting the lead content in urine by the triacid pretreatment inductively coupled plasma emission method is established, and a very satisfactory result is obtained by analyzing and comparing the freeze-dried human urine lead standard substance (GBW09104f) and the human urine sample by two methods.
Disclosure of Invention
The invention aims to solve the defects that the pretreatment process is complicated, lead loss or pollution is easily caused, and the accuracy of the result is greatly influenced in the prior art, and provides a method for measuring urinary lead by an inductively coupled plasma atomic emission spectrometry.
The method for measuring the urinary lead by the inductively coupled plasma atomic emission spectrometry comprises the following steps:
step 1, preparing a standard lead solution: preparing a plurality of fresh morning urine of healthy people with the same volume, respectively adding the fresh morning urine into a triangular beaker, adding a 65-68% nitric acid solution, evaporating the nitric acid solution at a low temperature until the volume of the fresh morning urine is 1/4-1/6 times that of the fresh morning urine, adding a 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down the urine, cooling, rinsing the wall of the beaker with deionized water, adding a 36-38% hydrochloric acid solution, heating and boiling to obtain a matrix solution, and respectively adding lead solutions with different contents into the matrix solution to prepare lead standard series solutions with different concentrations;
step 2, establishing a standard curve: preparing an inductively coupled plasma atomic emission spectrometer, sucking a lead standard series solution containing a human urine matrix into the inductively coupled plasma atomic emission spectrometer under the working condition of the inductively coupled plasma atomic emission spectrometer, respectively measuring the characteristic spectral line intensity of lead element, and drawing a standard curve by taking the concentration of the lead element as an abscissa and the characteristic spectral line intensity of the lead element as an ordinate after deducting the background spectral line intensity;
step 3, pretreatment of the urine sample: adding fresh morning urine of a person to be detected involved in lead activities into a triangular beaker, adding a 65-68% nitric acid solution, evaporating at a low temperature until the volume of the fresh morning urine is 1/4-1/6 times that of the fresh morning urine, adding a 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down and cooling, rinsing the wall of the beaker with deionized water, adding a 36-38% hydrochloric acid solution, heating and boiling, and controlling the volume;
step 4, detecting the spectral intensity: and (3) moving the urine into a colorimetric tube, detecting by using an inductively coupled plasma atomic emission spectrometer, and obtaining the final concentration of lead in the urine by corresponding the obtained spectral intensity result to a standard curve.
Preferably, the fresh morning urine is prepared in no less than three portions in step 1.
Preferably, the low-temperature evaporation temperature in the step 1 and the step 3 is 150-200 ℃, and the cooling temperature is 20-40 ℃.
Preferably, the volume of the urine after boiling in the step 3 is controlled to be smaller than the volume of the colorimetric tube in the step 4.
Preferably, the volume ratio of the fresh morning urine, the nitric acid solution, the perchloric acid solution and the hydrochloric acid solution in the steps 1 and 3 is (90-110): (9-11): (5-6): (2-3).
According to the invention, a three-acid pretreatment method of a nitric acid solution, a perchloric acid solution and a hydrochloric acid solution is adopted for fresh morning urine, the content of lead in the urine is detected by combining an inductively coupled plasma emission spectrometry, the content of lead is in a linear relation within the range of 0.1-10 ug/ml, the standard recovery rate is 96.2-106.2%, the relative standard deviation is lower than 8.49%, and a high-precision result is obtained by comparing with a dithizone spectrophotometry. The method for detecting the content of the lead in the urine by the triacid pretreatment inductively coupled plasma emission method has the advantages of high analysis speed, high sensitivity, good precision and the like, can better meet the test requirement of the content of the lead in the urine, and is worthy of popularization.
Drawings
FIG. 1 is a graph of the concentration of a standard lead solution of the present invention as a function of spectral intensity.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Examples
The invention provides a method for measuring urinary lead by an inductively coupled plasma atomic emission spectrometry, which comprises the following steps:
step 1, preparing a standard lead solution: taking 100ml of fresh urine of four healthy people respectively, adding into a 250ml triangular beaker respectively, adding 10ml of 65-68% nitric acid solution, evaporating at 150-200 ℃ until the volume of the solution is 25ml, adding 5ml of 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, cooling after the white smoke is completely dispersed, cooling at 20-40 ℃, then 2ml to 3ml deionized water is used for moistening and washing the wall of the beaker, 2ml to 3ml hydrochloric acid solution with the concentration of 36 percent to 38 percent is added, the beaker is heated to 100 ℃ and boiled, the solution is used as a matrix solution for preparing lead standard series solutions, then lead solutions with different contents are respectively added into the matrix solution to prepare lead standard series solutions with different concentrations, wherein the volume ratio of the fresh morning urine to the nitric acid solution to the perchloric acid solution to the hydrochloric acid solution is (90-110): (9-11): (5-6): (2-3);
step 2, establishing a standard curve: preparing an inductively coupled plasma atomic emission spectrometer, sucking a lead standard series solution containing a human urine matrix into the inductively coupled plasma atomic emission spectrometer according to specific working parameters of the inductively coupled plasma atomic emission spectrometer as shown in the following table 1, respectively measuring the characteristic spectral line intensity of lead, deducting the background spectral line intensity, and drawing a standard curve by taking the concentration of the lead as an abscissa and the characteristic spectral line intensity of the lead as an ordinate, wherein the standard curve is shown in fig. 1;
| parameter(s) | Numerical value |
| Plasma power/W | 1400 |
| Peristaltic pump speed/(Rpm) | 30 |
| Atomizer flow/(L/min) | 0.8 |
| Cooling air flow/(L/min) | 12.5 |
| Auxiliary gas flow/(L/min) | 0.8 |
| Sample rinsing time/s | 30 |
| Integration time/s | 28 |
| Carrier gas pressure (Mpa) | 0.8 |
TABLE 1
Taking 1% HNO3 as a medium, taking the treated healthy human urine as a substrate, and preparing four parts of standard series lead solutions respectively of 0 mug/ml, 0.1 mug/ml, 1.0 mug/ml and 10 mug/ml for measurement on an inductively coupled plasma atomic emission spectrometer. From fig. 1, it can be seen that the lead concentration is in a range of 1-10 μ g/l, the linear relationship is good, the correlation coefficient r2=0.9998, the correlation coefficient refers to the number of the linear relationship between the standard lead solution concentration and the spectral intensity, the closer the number is to 1, the more relevant the two variables are, i.e. the linear relationship of the standard curve is better, and the relationship between the standard lead solution concentration and the spectral intensity is as shown in table 2:
| standard series of serial numbers | Concentration (ug/ml) | Spectral intensity (cps) |
| S0 | 0 | 124 |
| S1 | 0.1 | 1308 |
| S2 | 1.0 | 17210 |
| |
10 | 200184 |
TABLE 2
Step 3, pretreatment of the urine sample: taking 100ml of fresh morning urine of a person to be detected who involves lead activities, adding the fresh morning urine into a 250ml triangular beaker, adding 10ml of a 65-68% nitric acid solution, evaporating at a low temperature of 150-200 ℃ until the volume of the solution is 25ml, adding 5ml of a 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down and cooling after the white smoke is dissipated, using 2 ml-3 ml deionized water to rinse the wall of the beaker, adding 2 ml-3 ml of a 36-38% hydrochloric acid solution, heating to 100 ℃ and boiling, and controlling the volume, wherein the volume ratio of the fresh morning urine to the nitric acid solution to the perchloric acid solution to the hydrochloric acid solution is (90-110): (9-11): 5-6): 2-3), and the healthy human urine is used as a matrix solution because the healthy human urine does not contain lead, but other components are as follows: the components such as inorganic salt, protein, uric acid and the like are not greatly different from those of a person to be detected, so that the lead-free gas detection device can be used as a lead standard substrate to ensure that the components of a standard sample are consistent with those of the sample to be detected except lead, so that the interference of detection of an inductively coupled plasma atomic emission spectrometer is small, and the person to be detected who is involved in lead activities is a person who is in contact with lead, including workers on factories related to the lead field and persons who breathe a large amount of lead-containing air due to lead contained in automobile exhaust can be used as the person to be detected;
step 4, detecting the spectral intensity: transferring the urine with the volume controlled smaller than 10ml into a 10ml colorimetric tube, detecting by using an inductively coupled plasma atomic emission spectrometer, and obtaining the final concentration of lead in the urine by corresponding the obtained spectrum intensity result to a standard curve;
the results of the different analytical methods carried out finally are compared in the following table 3:
TABLE 3
Table 3 shows the result comparison of different analysis methods, and it can be seen from the analysis results that the errors of the analysis results of different analysis methods meet the requirements, and the repeatability of the analysis result of each analysis method meets the requirements, indicating the accuracy of the method;
wherein: the X urine sample is a fresh morning urine sample of a lead-involved staff, and the freeze-dried human urine is purchased from the occupational health and poisoning control institute (the standard value is 0.022 ug/ml) of the Chinese disease control center;
the accuracy and precision of the assay results are shown in table 4 below:
TABLE 4
The standard samples, namely human urine, were added with lead standard solutions at concentrations of 0.010. mu.g/ml, 0.030. mu.g/ml and 0.040. mu.g/ml, and the measurement was carried out under the selected instrument conditions. The results are shown in Table 4, and according to the results, the recovery rate of the method in the standard addition is 96.2-106.2%, and the relative standard deviation is lower than 8.49%, which indicates that the method has high sensitivity and good reproducibility.
Urine samples are complex in matrix and contain large amounts of inorganic salts and organic components that can cause serious interference with the measurement, thus requiring pretreatment of the urine sample. The analysis method adopts triacid to process the urine sample, and the inductively coupled plasma spectrometry is used for determination, so that the recovery rate and the precision both meet the standard requirements of related detection methods, and the method is suitable for daily detection of batch samples.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The method for measuring the urinary lead by the inductively coupled plasma atomic emission spectrometry is characterized by comprising the following steps of:
step 1, preparing a standard lead solution: preparing a plurality of fresh morning urine of healthy people with the same volume, respectively adding the fresh morning urine into a triangular beaker, adding a 65-68% nitric acid solution, evaporating the nitric acid solution at a low temperature until the volume of the fresh morning urine is 1/4-1/6 times that of the fresh morning urine, adding a 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down the urine, cooling, rinsing the wall of the beaker with deionized water, adding a 36-38% hydrochloric acid solution, heating and boiling to obtain a matrix solution, and respectively adding lead solutions with different contents into the matrix solution to prepare lead standard series solutions with different concentrations;
step 2, establishing a standard curve: preparing an inductively coupled plasma atomic emission spectrometer, sucking a lead standard series solution containing a human urine matrix into the inductively coupled plasma atomic emission spectrometer under the working condition of the inductively coupled plasma atomic emission spectrometer, respectively measuring the characteristic spectral line intensity of lead element, and drawing a standard curve by taking the concentration of the lead element as an abscissa and the characteristic spectral line intensity of the lead element as an ordinate after deducting the background spectral line intensity;
step 3, pretreatment of the urine sample: adding fresh morning urine of a person to be detected involved in lead activities into a triangular beaker, adding a 65-68% nitric acid solution, evaporating at a low temperature until the volume of the fresh morning urine is 1/4-1/6 times that of the fresh morning urine, adding a 70-72% perchloric acid solution, emitting white smoke until the urine is clear and transparent, taking down and cooling, rinsing the wall of the beaker with deionized water, adding a 36-38% hydrochloric acid solution, heating and boiling, and controlling the volume;
step 4, detecting the spectral intensity: and (3) moving the urine into a colorimetric tube, detecting by using an inductively coupled plasma atomic emission spectrometer, and obtaining the final concentration of lead in the urine by corresponding the obtained spectral intensity result to a standard curve.
2. The method for measuring urinary lead by inductively coupled plasma atomic emission spectrometry according to claim 1, wherein the preparation of fresh morning urine in step 1 is not less than three.
3. The method for measuring urinary lead by using the inductively coupled plasma atomic emission spectrometry as claimed in claim 1, wherein the low-temperature evaporation temperature in the steps 1 and 3 is 150 ℃ to 200 ℃, and the cooling temperature is 20 ℃ to 40 ℃.
4. The method for measuring urinary lead by inductively coupled plasma atomic emission spectrometry according to claim 1, wherein the control volume in step 3 is that the volume of the boiled urine is smaller than the volume of the colorimetric cylinder in step 4.
5. The method for measuring the urinary lead by the inductively coupled plasma atomic emission spectrometry as claimed in claim 1, wherein the volume ratio of the fresh morning urine, the nitric acid solution, the perchloric acid solution and the hydrochloric acid solution in the steps 1 and 3 is (90-110): (9-11): (5-6): (2-3).
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