GB/T 39804-2021 PDF English
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GB/T 39804-2021: Method for determination of leachable harmful substances in wall materials---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT39804-2021
(Method for determination of leaching harmful substances in wall materials)
ICS 91.100.01
Q04
National Standards of People's Republic of China
Method for determination of leaching harmful substances in wall materials
Released on 2021-03-09
2021-10-01 implementation
State Administration of Market Supervision and Administration
Issued by the National Standardization Management Committee
Table of Contents
Foreword Ⅲ
1 Scope 1
2 Normative references 1
3 Instrument 1
4 Determination 1
5 Result calculation 2
Appendix A (normative appendix) Preparation method of leachate 4
Appendix B (Normative Appendix) Determination of the content of heavy metal elements in the leachate by inductively coupled plasma emission spectrometry
(ICP-OES) 5
Appendix C (Normative Appendix) Determination of the content of heavy metal elements in the leaching solution Inductively coupled plasma mass spectrometry (ICP-MS) 10
Appendix D (Normative Appendix) Determination of the content of heavy metal elements in the leachate Graphite Furnace Atomic Absorption Spectrometry (GFAAS) 14
Appendix E (Normative Appendix) Determination of the content of heavy metal elements in the leachate Flame Atomic Absorption Spectrometry (FAAS) 17
Appendix F (Normative Appendix) Determination of Heavy Metal Element Content in Leachate Atomic Fluorescence Method (AFS) 19
Appendix G (Normative Appendix) Determination of the content of hexavalent chromium in the leachate Spectrophotometry 21
Appendix H (Normative Appendix) Determination of the content of hexavalent chromium in the leachate by ion chromatography 23
Appendix I (Normative appendix) Determination of anion content in the leachate ion chromatography 25
Appendix J (Normative Appendix) Determination of pH Value of Extract 28
Appendix K (Normative Appendix) Determination of total soluble solids in the leachate 29
Appendix L (Normative Appendix) Determination of Chemical Oxygen Demand (COD) in the Leachate 31
Appendix M (Normative appendix) Determination of formaldehyde content in leachate spectrophotometric method 33
Appendix N (informative appendix) The scope of application of heavy metal element detection methods 36
Preface
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Building Materials Federation.
This standard is under the jurisdiction of the National Standardization Technical Committee for Building Materials for Walls, Roofs and Roads (SAC/TC285).
Drafting organizations of this standard. China Building Materials Inspection and Certification Group Xi’an Co., Ltd., Guangzhou Building Materials Industry Research Institute Co., Ltd., Xi’an
Ann Wall Materials Research and Design Institute Co., Ltd., Guizhou Building Material Product Quality Inspection and Testing Institute, Dalian Institute of Metrology, Inspection and Testing Co., Ltd.
Division, Guangxi Jianhong Construction Engineering Quality Inspection Co., Ltd., China Building Materials Inspection and Certification Group Guizhou Co., Ltd., Xuzhou Hongda Civil Engineering
Laboratory Co., Ltd., Zhejiang Fangyuan Building Material Co., Ltd., Jiangsu Construction Engineering Building Material Quality Inspection Center Co., Ltd., Agilent Technologies (China
China) Co., Ltd., Zhejiang Zhongyue Environmental New Materials Co., Ltd., China Building Materials Inspection and Certification Group Xuzhou Co., Ltd., Yunnan Hexin Engineering
Testing Consulting Co., Ltd., Jinhua Shuntong Environmental Construction Co., Ltd., Tangshan Honglin Silicone Co., Ltd., Haiyan Dabel New Building Materials
Co., Ltd., Huai'an Construction Engineering Quality Inspection Center Co., Ltd., and Steel Research Nac Inspection Technology Co., Ltd.
The main drafters of this standard. Li Wen, Jiang Deyong, Li Guiqiang, Quan Zonggang, Lin Ling, Wang Haibo, Su Yanjuan, Cao Yushu, Liu Jianyong, Cui Jinhua,
Tang Baoquan, Zhang Guihong, Wu Xin, Liu Tianjiao, Lu Meng, Peng Jianjun, Liu Xiaowen, Wu Zonggang, Cui Shouchen, Zhang Wenguang, Wang Tao, Mei Guozheng, Wang Meichun,
Liu Yonggan, Li Jiangfeng, Dong Lin, Cui Jin, Wei Youjun, Lu Shouping, Ding Baizhan, Qu Huayang.
Method for determination of leaching harmful substances in wall materials
Warning---Personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues
question. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This standard specifies the heavy metal elements, hexavalent chromium, anions, pH value, total soluble solids, chemical oxygen demand and formaldehyde in wall materials
Preparation and determination methods of the leaching solution.
This standard applies to wall materials that can leach heavy metal elements, hexavalent chromium, anions, pH, total soluble solids, and chemical oxygen demand
And formaldehyde determination. Roofing materials and road building materials can be implemented with reference to this standard.
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 601-2016 Preparation of chemical reagent standard titration solution
GB/T 6682-2008 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
GB/T 12805-2011 Laboratory glass burette
GB/T 12806-2011 Laboratory glassware single mark volumetric flask
GB/T 12808-2015 Laboratory glass instrument single mark pipette
3 Instruments
3.1 Electronic balance
Sensitivity is 0.1mg and 0.01g.
3.2 Burette
It meets the requirements of Grade A in GB/T 12805-2011.
3.3 Single mark volumetric flask
Meet the requirements of Class A in GB/T 12806-2011.
3.4 Single marking pipette
It meets the requirements of Grade A in GB/T 12808-2015.
4 Determination
4.1 Preparation of the extract
Proceed in accordance with the provisions of Appendix A.
4.2 Determination of the content of heavy metal elements in the leaching solution
4.2.1 The inductively coupled plasma emission spectroscopy method shall be carried out in accordance with the provisions of Appendix B.
4.2.2 Inductively coupled plasma mass spectrometry should be carried out in accordance with Appendix C.
4.2.3 Graphite furnace atomic absorption spectrometry shall be carried out in accordance with Appendix D.
4.2.4 The flame atomic absorption spectrometry is carried out in accordance with the provisions of Appendix E.
4.2.5 The atomic fluorescence method shall be carried out in accordance with the provisions of Appendix F.
4.3 Determination of hexavalent chromium content in the leaching solution
4.3.1 The spectrophotometry shall be carried out in accordance with the provisions of Appendix G.
4.3.2 Ion chromatography shall be carried out in accordance with the provisions of Appendix H.
4.4 Determination of the content of anions (F-, Cl-, NO-3, SO2-4) in the leachate
Proceed in accordance with the provisions of Appendix I.
4.5 Determination of the pH value of the extract
Proceed in accordance with the provisions of Appendix J.
4.6 Determination of total soluble solids content in the extract
Follow the provisions of Appendix K.
4.7 Determination of Chemical Oxygen Demand (COD) in the Leachate
Follow the provisions of Appendix L.
4.8 Determination of formaldehyde content in leachate
Proceed in accordance with the provisions of Appendix M.
4.9 The scope of application of heavy metal element detection methods
See Appendix N.
5 Result calculation
5.1 Appendix B, Appendix E, Appendix G, Appendix I, Appendix K, Appendix L and Appendix M determine the content of leaching hazardous substances in the samples
Formula (1) calculation.
wi=
Xi×200
(1)
Where.
wi --- the content of the leaching hazardous substance i in the sample, in milligrams per kilogram (mg/kg);
Xi --- the content of harmful substance i in the extract, in milligrams per liter (mg/L);
200---The total volume of the extract, in milliliters (mL);
m ---The mass of the sample, in grams (g).
5.2 The content of leaching hazardous substances in the samples measured in Appendix C, Appendix D, Appendix F, and Appendix H is calculated according to formula (2).
wi=
Xi×200
(2)
Where.
wi --- The content of the leaching hazardous substance i in the sample, in micrograms per kilogram (μg/kg);
Xi --- the content of harmful substance i in the extract, in micrograms per liter (μg/L);
200---The total volume of the extract, in milliliters (mL);
m ---The mass of the sample, in grams (g).
5.3 The results obtained should be rounded up in accordance with GB/T 8170, with 1 decimal place, if the entrusting party or relevant standards require otherwise, according to the required digits.
Number of rounds.
Appendix A
(Normative appendix)
Preparation method of leachate
A.1 Method summary
At (23±2)℃ room temperature, soak the sample in water (ground to powder), stir on a magnetic stirrer for 8h and then continue to stand for 64h, soak
The effluent passes through a 0.45μm filter membrane.
A.2 Water
Meet the secondary water requirements specified in GB/T 6682-2008.
A.3 Equipment
A.3.1 Magnetic stirrer.
A.3.2 Filter device, pressure filter device or vacuum filter device, the leachate that is not easy to filter can be separated by a centrifuge.
A.3.3 Filter membrane, 0.45μm.
A.3.4 Desiccator, equipped with color-changing silica gel.
A.4 Sample preparation
Take a sample of no less than 4kg, crush it to less than 5mm, and divide it into quarters to obtain a 500g sample, and then grind it until all the samples pass.
Pass through an 80μm square-hole sieve, mix well, put it into a clean, dry sample bottle, store it in a desiccator (A.3.4), and set aside.
A.5 Experimental procedure
Weigh 100g sample, accurate to 0.1mg, place it in a 500mL glass beaker, add.200.0mL water (A.2), and put a
Stir the magnet and seal the mouth of the beaker with a parafilm. Place the beaker on a magnetic stirrer and stir, stir at (23±2)℃ room temperature for 8h, then continue
Let it stand for 64h and filter through the filter device (A.3.2) to obtain the leachate. The leaching solution should complete the experiment within 24h.
Do a blank experiment at the same time.
10mg/L, 25mg/L, 50mg/L standard working solution, the medium is nitric acid solution (B.3.6).
B.4.2.8 If the standard working solution has turbidity, precipitation or color change, it should be re-prepared.
B.5 Apparatus
Inductively coupled plasma emission spectrometer (ICP-OES) and its corresponding auxiliary equipment.
B.6 Analysis steps
B.6.1 Acidity adjustment of the leaching solution
Use nitric acid solution (B.3.4) to adjust the acidity of the extract to be consistent with the acidity of the standard working solution.
B.6.2 Drawing of standard working curve
Set the analysis conditions of the instrument according to the test requirements and instrument conditions, ignite the plasma, and wait for the plasma torch to stabilize, at the corresponding wavelength
Next, measure the spectral intensity of each metal element in the standard working solution in B.4.2 in the order of concentration from low to high. With heavy metal content
It is the abscissa and the spectral intensity is the ordinate to draw the standard working curve.
B.6.3 Determination of heavy metal elements in the leaching solution
Set the analysis conditions of the instrument according to the test requirements and instrument conditions, ignite the plasma, and wait for the plasma torch to stabilize. Selection and criteria
The working solution is measured under the same instrument conditions, and the spectral intensity of each heavy metal element in the leaching solution and the blank leaching solution are measured separately.
The corresponding heavy metal element content (ci) of the leachate and the corresponding heavy metal element content (ci0) of the blank leachate are found in the curve. If in the leaching solution
The content of heavy metal elements exceeds the calibration curve range, and the leaching solution needs to be properly diluted to make the acidity consistent with that before the dilution.
Set, the dilution factor is F.
B.7 Result calculation
B.7.1 The content of heavy metal element i in the leaching solution is calculated according to formula (B.1).
Xi=(ci-ci0)×F (B.1)
Where.
Xi --- the content of heavy metal element i in the leachate, in milligrams per liter (mg/L);
ci --- the content of heavy metal element i found on the standard working curve, in milligrams per liter (mg/L);
ci0 --- The content of heavy metal element i in the blank leachate found on the standard working curve, in milligrams per liter (mg/L);
F ---Dilution multiple, the ratio of the volume after dilution to the aliquoted volume.
B.7.2 Take the arithmetic average of the two test results as the test result. The result obtained should be rounded according to GB/T 8170, when the result is ≥1mg/L
When the time, keep 1 decimal place; when the result is less than 1mg/L, keep 2 decimal places, if the entrusting party or relevant standards require otherwise, according to the required digits
Amendment.
B.8 Precision
B.8.1 Repeatability
In the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same object under test in a short period of time.
The relative deviation of the two independent test results obtained by independent tests is less than 5%.
B.8.2 Reproducibility
In different laboratories, different operators use different equipment, according to the same test method, independently conduct the same test object.
The relative deviation of the two independent test results obtained by the line test is less than 10%.
It should be considered that the mass concentration of internal standard elements in the analysis solution is about 5μg/L~50μg/L.
C.4.4 Tuning solution
This solution is used for instrument tuning and quality calibration before analysis. The solution must contain enough heavy metal ions to cover the entire mass spectrum.
It is advisable to use metal elements containing (Li)Be, Mn, Co, Y, In(Tl) and Pb as the tuning solution. You can directly purchase a certified standard solution and use nitric acid.
The solution (B.3.6) is diluted. (The mass number and concentration of each metal element in the tuning solution required for the tuning of each instrument may be different. For details, please follow
(Tune in the respective laboratory conditions to ensure that the instrument is in normal state)
C.5 Instruments
Inductively coupled plasma mass spectrometer (ICP-MS) and its corresponding auxiliary equipment.
Instrument working conditions. Different types of instruments have different optimal working conditions. Standard mode, collision mode, reaction cell mode, etc. should be in accordance with the instrument
The operation manual of the device.
C.6 Analysis steps
C.6.1 Adjust the acidity of the leaching solution
Use nitric acid solution (B.3.4) to adjust the acidity of the extract to be consistent with the acidity of the standard working solution.
C.6.2 Instrument tuning
After igniting the plasma, the instrument needs to be warmed up and stabilized for 30 minutes. First, use the mass spectrometer to tune the sensitivity of the solution to the instrument, the oxide and the double
The charge is tuned. Under the condition that the above indicators meet the requirements, the relative standard deviation of the signal intensity of the metal elements contained in the tuning solution
The difference is ≤5%. Then perform quality correction and resolution verification within the quality range covering heavy metal elements, such as the quality correction result and the true value
The difference exceeds ±0.1amμ or the resolution of the tuning metal element signal is greater than 0.6amμ~0.8amμ at 10% peak height.
The range of the mass spectrometer should be calibrated in accordance with the requirements of the instrument manual.
C.6.3 Drawing of standard working curve
Set the analysis conditions of the instrument according to the test requirements and instrument conditions. After the instrument is stable, determine the concentration in the order from low to high. C.4.1
Medium standard working solution. The internal standard solution can be directly added to the standard working solution, or it can be automatically added by the peristaltic pump before the analysis solution is atomized.
Into. The concentration of heavy metal solution is taken as the abscissa, and the ratio of the heavy metal element signal to the internal standard signal is taken as the ordinate to establish a calibration curve.
The linearity of the standard working curve is checked by calculating the correlation coefficient, which should be greater than 0.999.
C.6.4 Determination of heavy metal elements in the leaching solution
When the sample is measured, the same amount of internal standard element standard solution as when the standard working curve is drawn should be added.
Before the measurement of each sample, flush the system with nitric acid solution (B.3.6) until the signal is reduced to the minimum, and start after the analysis signal is stable
Determination. Select the same instrument conditions as the standard working solution to determine the information of each heavy metal element in the leaching solution and the blank leaching solution.
No. ratio, find the corresponding heavy metal element content (ci) of the leachate and the corresponding heavy metal element content of the blank leachate in the standard working curve
(ci0). If the content of heavy metal elements in the leachate exceeds the calibration curve range, it needs to be diluted with a nitric acid solution (B.3.6) and re-measured. Dilution times
The number is F.
C.7 Result calculation
C.7.1 The content of heavy metal element i in the leachate is calculated according to formula (C.1).
Xi=(ci-ci0)×F (C.1)
Where.
Xi --- the content of heavy metal element i in the leachate, in micrograms per liter (μg/L);
ci --- the content of heavy metal element i found on the standard working curve, in micrograms per liter (μg/L);
ci0 --- The content of heavy metal element i in the blank leachate found on the standard working curve, in micrograms per liter (μg/L);
F ---Dilution multiple, the ratio of the volume after dilution to the aliquoted volume.
C.7.2 Take the arithmetic average of the two test results as the test result. The result should be rounded according to GB/T 8170, when the result is ≥1μg/L
When the time, keep 1 decimal place; when the result is < 1μg/L, keep 2 decimal places, if the entrusting party or relevant standards require otherwise, according to the required digits
Amendment.
C.8 Precision
C.8.1 Repeatability
In the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same object under test in a short period of time.
The relative deviation of the two independent test results obtained by independent tests is less than 10%.
C.8.2 Reproducibility
In different laboratories, different operators use different equipment, according to the same test method, independently conduct the same test object.
The relative deviation of the two independent test results obtained by the line test is less than 20%.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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