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SN/T 1732.24-2020: (Pyrotechnic composition for fireworks and firecrackers - Part 24: Determination of arsenic content-Atomic fluorescence method)
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(Pyrotechnic composition for fireworks and firecrackers - Part 24: Determination of arsenic content-Atomic fluorescence method)
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SN/T 1732.24-2020
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Basic data | Standard ID | SN/T 1732.24-2020 (SN/T1732.24-2020) | | Description (Translated English) | (Pyrotechnic composition for fireworks and firecrackers - Part 24: Determination of arsenic content-Atomic fluorescence method) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | A80 | | Classification of International Standard | 11.100 | | Word Count Estimation | 7,784 | | Date of Issue | 2020-08-27 | | Date of Implementation | 2021-03-01 | | Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] | | Issuing agency(ies) | General Administration of Customs | SN/T 1732.24-2020: (Pyrotechnic composition for fireworks and firecrackers - Part 24: Determination of arsenic content-Atomic fluorescence method)
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Pyrotechnic composition used for fireworks- Part 24.
Determination of arsenic content-Atomic fluorescence spectrometry (AFS)
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Pyrotechnic composition for fireworks and firecrackers. Part 24.Determination of arsenic content. Atomic fluorescence method
2020-08-27 release
2021-03-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
SN/T 1732 "Pyrotechnic Reagent for Fireworks and Firecrackers" is divided into the following 24 parts.
--Part 1.Determination of barium content;
--Part 2.Determination of dichromate content;
--Part 3.Determination of zinc content;
--Part 4.Determination of copper content;
--Part 5.Determination of titanium content;
--Part 6.Determination of strontium content;
--Part 7.Determination of lead content;
--Part 8.Determination of sodium content;
--Part 9.Determination of magnesium content;
--Part 10.Determination of sulfur content;
--Part 11.Determination of potassium content;
--Part 12.Determination of red phosphorus content;
--Part 13.Determination of Boric Acid Content;
--Part 14.Qualitative detection method of dextrin;
--Part 15.Detection method of polyvinyl chloride;
--Part 16.Picric acid detection method high performance liquid chromatography;
--Part 17.Detection method of hexachlorobenzene gas chromatography;
--Part 18.Detection method of chlorinated paraffin;
--Part 19.Detection method of gallic acid by high performance liquid chromatography;
--Part 20.Determination of barium content by flame atomic absorption method;
--Part 21.Determination of lead content by flame atomic absorption spectrometry;
--Part 22.Qualitative detection of lead, chromium, cadmium, mercury and arsenic by energy dispersive X-ray fluorescence spectrometry;
--Part 23.Determination of lead, chromium, cadmium, mercury and arsenic content by inductively coupled plasma emission spectrometry;
- Part 24.Determination of Arsenic Content Atomic Fluorescence Method.
This part is part 24 of SN/T 1732.
This part was drafted in accordance with the rules given in GB/T 1.1-2020.
This part is proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organization of this section. Nanning Customs of the People's Republic of China.
The main drafters of this section. Shang Jie, Huang Chengxing, Peng Xiaofeng, Yan Chun, Xiao Huanxin.
Pyrotechnics for fireworks and firecrackers Part 24.
Determination of arsenic content Atomic fluorescence method
Warning. The personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues
It is the responsibility of the user to adopt appropriate safety and health measures and to ensure compliance with the conditions stipulated by relevant national laws. Involved in this standard
Pyrotechnics is a kind of flammable and explosive dangerous goods. The following are the most important safety technical regulations.
a) The preparation of the sample should be carried out under the conditions of safety protection measures;
b) The preparation and storage of the sample should not exceed the conditions allowed by the safety protection;
c) The sample should be dried in a safe explosion-proof drying box, and the drying temperature should not exceed 55°C;
d) The remaining samples and the tested samples should be destroyed in time.
1 Scope
This section specifies the method for the determination of arsenic in pyrotechnics for fireworks and firecrackers.
This section applies to the determination of arsenic content in pyrotechnics for fireworks and firecrackers. Measuring range. arsenic content (calculated by mass fraction of arsenic)
Greater than 0.1%.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Principle
After the sample is properly pretreated, it is nitrified with nitric acid and hydrogen peroxide, and digested with atmospheric pressure microwave. The pentavalent arsenic that may exist in the sample
Use thiourea or ascorbic acid to reduce to trivalent arsenic, then use potassium borohydride (sodium) to reduce the arsenic ion to arsine, and use argon to reduce the arsine
It is loaded into the quartz atomizer and decomposed into atomic arsenic, which is excited by the emission light of the arsenic hollow cathode lamp to produce atomic fluorescence.
Under fixed conditions, the degree is proportional to the concentration of arsenic in the test solution, and it can be quantitatively detected in comparison with the standard series.
4 Reagents and materials
Unless otherwise specified, only use reagents confirmed to be analytically pure and at least Grade 3 water as specified in GB/T 6682.
4.1 Absolute ethanol.
4.2 Acetone. analytically pure, density 0.788 g/mL (25 ℃).
4.3 Nitric acid. pure superior grade, density 1.420 g/mL (25 ℃).
4.4 Nitric acid solution. Measure 100 mL of nitric acid (4.3) and add 500 mL of water to mix.
4.5 Hydrochloric acid. pure superior grade, density 1.189 g/mL (20 ℃).
4.6 30% hydrogen peroxide. density 1.111 g/mL (20 ℃).
4.7 10% ascorbic acid 10% thiourea mixture. weigh out 10.0 g of ascorbic acid and 10.0 g of thiourea, and dissolve it with 100 mL of water.
Equipped when used.
4.8 Potassium borohydride solution (1.0%). first weigh 0.5 g of potassium hydroxide into the water, and after it is completely dissolved, add the weighed
1.0 g potassium borohydride, dissolve and shake well, dilute to 100 mL, and prepare it when used.
4.9 Potassium hydroxide solution (100 g/L). First weigh 50 g of potassium hydroxide into the water, and after it is completely dissolved, dilute to 500 mL.
4.10 Hydrochloric acid solution (carrier fluid). Measure 100 mL of hydrochloric acid (4.5), and dilute to 1000 mL with water.
4.11 Arsenic standard solution (1 000 mg/L). purchase a commercially available certified standard material.
4.12 Arsenic standard solution (50 mg/L). accurately measure 5 mL of arsenic standard solution (4.11) and dilute to volume with hydrochloric acid solution (4.10)
100 mL.
4.13 Arsenic standard solution (1 mg/L). accurately measure 2 mL of arsenic standard solution (4.12), and dilute to volume with hydrochloric acid solution (4.10)
100 mL.
4.14 Arsenic standard solution (100 μg/L). accurately measure 5 mL of arsenic standard solution (4.13) and add 10 mL of 10% ascorbic acid
10% thiourea mixture (4.7), dilute to 50 mL with hydrochloric acid solution (4.10).
4.15 High purity argon. over 99.99%.
5 Instruments
5.1 Sand core crucible. No. 4.
5.2 Safety explosion-proof oven. room temperature ~ 250 ℃, temperature control accuracy is ± 2 ℃.
5.3 Analytical balance. the accuracy is 0.1 mg.
5.4 Atomic fluorescence spectrometer, arsenic hollow cathode lamp.
5.5 Atmospheric microwave digestion apparatus.
5.6 Generally commonly used laboratory instruments and equipment, glass instruments should be soaked in nitric acid solution (4.4) for more than 12 hours before use.
6 Preparation of samples
6.1 Prepare the sample in accordance with the provisions of Chapter 4 in GB/T 15813-1995.
6.2 After the sample is dried in a safety explosion-proof oven specified in 5.2 at 50 ℃ ~ 55 ℃ for 4 hours, it is placed in a desiccator to cool to room temperature.
7 Analysis steps
7.1 Preparation of test solution
7.1.1 Weigh 2.0 g sample (accurate to 0.1 mg), place it in a clean and dry No. 4 sand core crucible (5.1), use 100 mL
Water ethanol (4.1) was added to the sand core crucible (5.1) in 5 times to soak, filtered by suction, and then washed with 100 mL of acetone (4.2) in 5 times to wash the filter residue.
Let stand to make the absolute ethanol (4.1) and acetone (4.2) in the sand core crucible volatilize.
7.1.2 Transfer the remainder in the sand core crucible (5.1) to the digestion tank, rinse with a small amount of water, and add 3.0 mL of nitric acid (4.3)
Pre-digestion for 30 minutes, when the bubbles are not violently released, add 2.0 mL nitric acid (4.3) and 2.0 mL hydrogen peroxide (30%) (4.6).
Follow the set procedure for microwave digestion and acid removal.
7.1.3 After the end, take out and cool, transfer the digested sample to a 50 mL volumetric flask, rinse with ultrapure water several times, and measure into 5.0 mL
Hydrochloric acid (4.5), then add 10 mL of 10% ascorbic acid and 10% thiourea mixture (4.7), and dilute to the mark with ultrapure water.
Let stand for 30 min, shake well before testing.
7.2 Blank experiment
Prepare a blank solution according to step 7.1, and add hydrochloric acid (4.5), 10% ascorbic acid and 10% thiourea mixture (4.7).
7.3 Standard curve drawing
7.3.1 Preparation of series standard solution. automatically dilute the main standard solution 100 μg/L to 0 μg/L, 5 μg/L, 10 μg/L, 20 μg/L,
50 μg/L and 100 μg/L form a series of standard solutions.
7.3.2 Measurement of fluorescence of series standard solutions. start the atomic fluorescence spectrometer (5.4), make the instrument run fully and stably, select the instrument
The best test conditions for the device (see Appendix A). Inhale arsenic standard solution, potassium borohydride solution (4.8) and carrier fluid (4.10) in order,
Measure its fluorescence value.
7.3.3 Draw a standard curve. take the concentration of arsenic standard solution (μg/L) as the abscissa, and use the corresponding blank-corrected arsenic standard
The fluorescence intensity of the quasi-solution is plotted on the ordinate to obtain the standard curve.
7.4 Determination of test solution
According to the optimized test conditions of the standard curve, each test solution is tested 3 times, and a blank test is done under the same conditions.
8 Result calculation
The content of barium is expressed as the mass fraction w (mg/kg) of arsenic and calculated according to formula (1).
Where.
w --The mass fraction of arsenic, in milligrams per kilogram (mg/kg);
c1-the value of the concentration of arsenic in the test solution read from the standard curve, in micrograms per liter (μg/L);
c0 --The value of the concentration of arsenic in the blank solution read from the standard curve, in micrograms per liter (μg/L)
V-the value of the constant volume of the test solution, the unit is milliliters (mL);
m-the value of the mass of the sample, in grams (g);
f-Dilution factor.
The relative deviation of the two parallel determination results is not more than 10%, the result is the average of the two parallel determination results, and the result is expressed as
According to the rules of GB/T 8170, 3 significant digits are reserved.
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