Identification of leaching toxicity by inductively coupled plasma emission spectrometry (3)

(7) Analysis and testing

The pretreated sample and blank solution (the solution maintains 5% nitric acid acidity), under the best operating parameters of the instrument, in accordance with the relevant provisions of the instrument manual, after two points of standardization, do the sample and blank determination

1.

The samples are in accordance with "Solid Waste Leaching Toxicity Leaching Method Sulfuric Acid Nitric Acid Method" (HJ/T299), "Solid Waste Leaching Toxicity Leaching Method Acetic Acid Buffer Solution Method" (HJ/T300), "Solid Waste Leaching Toxicity Leaching Method Horizontal Oscillation Method" (HJ557 ) To prepare

Take the leaching solution as an example.

2.

The mass concentration of the standard substance corresponding to the measured signal value is drawn into a calibration curve, and the reference conditions are silver (Ag), aluminum (A1), arsenic (As), barium (Ba), beryllium (Be), and calcium (Ca) , Cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn), sodium (Na), nickel (Ni) The standard curve parameters of, lead (Pb), antimony (Sb), strontium (Sr), thorium (Th), titanium (Ti), thallium (mouth), vanadium (V), zinc (Zn) are shown in Table 5-19 , The correlation r value is not less than 0.

Table 5-19 Standard curve parameters

3.

According to the requirements of HJ/T299-2007, process 7 sets of extract blanks, and add all reagents of the same volume as in the sample processing process to evaluate the possible contamination during the sample preparation process

Note: All containers used in the measurement need to be cleaned, rinsed with 10% hot nitric acid , and then rinsed with tap water and deionized water repeatedly to minimize the blank background

Table 5-20 Blank test and detection limit statistics

4.

To verify the reliability of the method, this method can be used to determine the degree of mutual agreement of a set of measured values ​​of the same homogeneous sample

Table 5-21 Repeatability test results of samples

5.
Method accuracy

The uniformity of the sample and the chemical properties of the matrix will affect the recovery rate and data quality of the analyte.
Take several samples from the same sample and perform repeated analysis with the same conditions for standard addition and recovery to evaluate the accuracy of this type of analysis
.
For example, the standard addition recovery test is carried out on a solid waste sample leachate, and the standard addition recovery repeated measurement is performed 7 times under the same conditions.
The average recovery rate is between 80.
3% and 118% (see Table 5-22)
.

Table 5-22 Standard addition recovery test results

Related Links: Identification of Leaching Toxicity by Inductively Coupled Plasma Atomic Emission Spectrometry (2)