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GB/T 41330-2022: Analysis of water used in boiler and cooling system - Determination of trace copper, iron, sodium, calcium and magnesium - Inductively coupled plasma mass spectrometry (ICP-MS)
GB/T 41330-2022
Analysis of water used in boiler and cooling system - Determination of trace copper, iron, sodium, calcium and magnesium - Inductively coupled plasma mass spectrometry (ICP-MS)
ICS 13.060.50; 71.040.40
CCSG76
National Standards of People's Republic of China
Methods of Analysis for Boiler Water and Cooling Water
Determination of trace copper, iron, sodium, calcium, magnesium content
Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
tracecopper, iron, sodium, calcium and magnesium-Inductively
2022-03-09 Released 2022-10-01 Implementation
State Administration for Market Regulation
Released by the National Standardization Administration
Methods of Analysis for Boiler Water and Cooling Water
Determination of trace copper, iron, sodium, calcium, magnesium content
Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
WARNING. The strong acids used in this document are corrosive, avoid inhalation or contact with skin. If splashed, rinse immediately with plenty of water
Wash and seek medical attention immediately in severe cases.
1 Scope
This document describes the determination of trace copper, iron, sodium, calcium, magnesium content in boiler water and cooling water by inductively coupled plasma mass spectrometry.
This document is applicable to the determination of trace copper, iron, sodium, calcium and magnesium content in boiler water and cooling water. Measuring range. copper content
0.1μg/L~1000μg/L, iron content 5μg/L~1000μg/L, sodium content 10μg/L~1000μg/L, calcium content 10μg/L~
1000μg/L, magnesium content 1μg/L~1000μg/L, when it exceeds 1000μg/L, it should be diluted and measured.
2 Normative references
The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, dated citations
documents, only the version corresponding to that date applies to this document; for undated references, the latest edition (including all amendments) applies to
this document.
GB/T 602 Preparation of standard solutions for the determination of impurities in chemical reagents
GB/T 6041 General Rules for Mass Spectrometry Analysis Methods
GB/T 6907 Boiler Water and Cooling Water Analysis Method Water Sample Collection Method
GB/T 33087-2016 Specifications and test methods of high-purity water for instrumental analysis
GB/T 39486 General Rules for Inductively Coupled Plasma Mass Spectrometry Analysis of Chemical Reagents
3 Terms and Definitions
Terms and definitions defined in GB/T 6041 and GB/T 39486 apply to this document.
4 Method summary
The element to be measured in the sample solution is atomized by the atomization system to form an aerosol, which is brought into the plasma torch by the carrier gas, and is heated under high temperature and inert gas.
It is fully evaporated, dissociated, atomized and ionized in the body, and converted into positively charged ions, which enter the mass spectrometer through the ion collection system, and the mass spectrometer root
Separation is performed according to the mass-to-charge ratio (mass-to-charge ratio) of the ions. The mass spectral response value of each analyte is proportional to its concentration in the sample, so that
Quantitative analysis of each element.
5 Reagents or materials
Unless otherwise specified, only use reagents of superior grade and above.
5.1 Water. It complies with the provisions of high-purity water for instrumental analysis in GB/T 33087-2016.
5.2 The standard solution of impurities required in the test, if no other requirements are specified, shall be prepared according to the provisions of GB/T 602 or the commercially available standard shall be selected.
solution.
5.3 Nitric acid. Spectroscopically pure.
5.4 Hydrochloric acid. Spectroscopically pure.
5.5 Hydrochloric acid solution. 1 1.
5.6 Nitric acid solution. 1 1.
5.7 Nitric acid solution..199.
5.8 Copper standard stock solution I. 1000mg/L. Weigh 1.000g of metallic copper, accurate to 0.2mg. Add 50 mL of hydrochloric acid solution
Heat until all dissolved, cool and transfer to a 1000mL volumetric flask, dilute with water to the mark. Or use commercially available standard solutions.
5.9 Copper standard stock solution II. 100mg/L.
5.10 Iron standard stock solution I. 1000mg/L. Weigh 1.000g of metallic iron, accurate to 0.2mg. in 100 mL hydrochloric acid solution
After heating to complete dissolution, transfer to a 1000mL volumetric flask after cooling, and dilute to the mark with water. Or use commercially available standard solutions.
5.11 Iron standard stock solution II. 100mg/L.
5.12 Sodium standard stock solution I. 1000mg/L. Weigh 2.542g of standard chlorinated pre-burned at 500℃~600℃ to a constant amount
Sodium, accurate to 0.2mg, dissolved in water, transferred to a 1000mL volumetric flask, diluted with water to the mark, and shaken. Or use commercially available standard solutions.
5.13 Sodium standard stock solution II. 100mg/L.
5.14 Calcium standard stock solution I. 1000mg/L. Weigh 2.500g of premium pure carbonic acid pre-dried at 105℃~110℃ to a constant amount
Calcium, to the nearest 0.2 mg. Put it in a 100mL beaker, add 50mL water, 10mL hydrochloric acid, dissolve it and transfer it to a 1000mL volumetric flask
, dilute to volume with water, and shake well. Or use commercially available standard solutions.
5.15 Calcium standard stock solution II. 100mg/L.
5.16 Magnesium standard stock solution I. 1000mg/L. Weigh 1.660g of excellent grade pure oxide pre-fired at 800℃±50℃ to constant weight.
Magnesium, to the nearest 0.2 mg. Put it in a 100mL beaker, add a small amount of water to wet the sample, add 25mL hydrochloric acid, dissolve it and transfer it to
In a 1000mL volumetric flask, dilute to the mark with water and shake well. Or use commercially available standard solutions.
5.17 Magnesium standard stock solution II. 100mg/L.
5.18 Mixed standard stock solution. a certified mixed standard solution can be purchased, or it can be used according to the mutual interference between elements and the properties of the standard solution.
quality and the content of the element to be measured, the standard stock solution I or II of each element is divided into groups to prepare a mixed standard stock solution, and stored in a sealed polystyrene
in vinyl or polypropylene bottles.
5.19 Mixed standard solution. 10mg/L. Pipette 10.00mL copper, iron, sodium, calcium, magnesium standard stock solution II, put it in a 100mL volumetric flask
, dilute to the mark with nitric acid solution (1 99) and shake well. The solution is used now.
5.20 Internal standard standard stock solution. 10mg/L or 1mg/L, commercially available. 6Li, 45Sc, and 74Ge should be selected as internal standard elements, and the
See Appendix A for the selection of the internal standard corresponding to the mass number.
5.21 Internal standard standard solution. According to the requirements of the instrument manual, dilute the internal standard stock solution with nitric acid solution (1.99) to an appropriate concentration.
5.22 Mass spectrometer tuning solution. 1 μg/L or 10 μg/L, other concentrations recommended by the instrument manual can also be used. Lithium-containing
Standard solutions of elements (Li), yttrium (Y), beryllium (Be), magnesium (Mg), cobalt (Co), indium (In), thallium (Tl), lead (Pb) and bismuth (Bi) for mass spectrometer tuning
solution.
5.23 Argon gas. the purity is not less than 99.999%.
5.24 Helium. the purity is not less than 99.999%.
5.25 Microporous filter membrane. cellulose acetate filter membrane with a pore size of 0.45 μm.
6 Instruments and equipment
6.1 Inductively coupled plasma mass spectrometer (ICP-MS) should be equipped with collision/reaction cell.
6.2 Digestion equipment. temperature-controlled electric hot plate or microwave digestion apparatus or graphite digestion apparatus.
6.3 Sampling bottle. The material is high density polypropylene, high density polyethylene or fluorinated polyethylene propylene (FEP). The material of the bottle body and bottle cap should not be
Contains or can leach any analyte.
6.4 Beaker. The material is Teflon, 100mL or 250mL.
6.5 Volumetric flask. The material is polypropylene, fusible polytetrafluoroethylene (PFA) or quartz.
7 Test steps
7.1 General
7.1.1 Environmental requirements. the number of particles with a particle size of 0.5 μm or more in the instrument environment should be below 3.5×105 particles/m3, or according to the instrument manual.
installation condition control.
7.1.2 Unless otherwise specified, all glass and plastic containers used in the test shall be cleaned as follows.
a) Before use, the container needs to be soaked in nitric acid solution (199) for at least 24h;
b) Rinse with water at least three times.
7.1.3 The polyamide container shall not be soaked in acid.
7.1.4 The container containing the high concentration metal ion solution can no longer be used for the analysis and determination of trace elements.
7.2 Sampling method
Before sampling, add nitric acid solution (1 1) to the sampling bottle (add 1 mL of nitric acid solution (1 1) for every 100 mL of water sample), and after taking the water sample
Shake immediately. The acidity of the water sample after acidification should be consistent with the calibration curve solution. Alkaline water samples can increase the amount of acid, so that the pH value of the sample is less than 2.0.
The collection method and storage of water samples shall comply with the provisions of GB/T 6907.
7.3 Sample Preparation
7.3.1 When there are many suspended solids in the water sample, use a 0.45 μm filter membrane to filter, discard the initial 50 mL of filtrate, and wash the sample with a small amount of filtrate.
The filtrate is collected and stored in a sampling bottle, and the sample can be placed for 14 days.
7.3.2 When the content of chemical oxygen demand (COD) in the sample is greater than 100 mg/L, 40 mL (or depending on the concentration of the element to be measured in the sample) should be accurately removed.
Add 2.0 mL of nitric acid and 1.0 mL of hydrochloric acid to the water sample in a polytetrafluoroethylene beaker, cover with a watch glass, and heat to a slight boil for about 30 min.
until the digestion is complete; or place the acid-added sample in a digestion tank and digest it at 150 °C for 30 min on a microwave digestion apparatus or graphite digestion apparatus.
Transfer to a 50mL volumetric flask, make up to the mark with water, and shake well. Blank test solutions were prepared in the same manner.
7.4 Preparation of calibration solutions
7.4.1 According to the content range of the element to be measured in the sample, select the appropriate calibration solution series.
7.4.2 Pipette an appropriate amount of mixed standard solution and place it in 8 100mL volumetric flasks, dilute it to the mark with nitric acid solution (1.99), shake well, and get
Concentrations of 0.0μg/L, 5.0μg/L, 10.0μg/L, 20.0μg/L, 40.0μg/L, 60.0μg/L, 80.0μg/L, 100.0μg/L
Low concentration series of calibration solutions.
7.4.3 Pipette an appropriate amount of mixed standard solution and place it in 8 100mL volumetric flasks, dilute it with nitric acid solution (1.99) to the mark, shake well, and get
To high concentrations of 0μg/L, 50μg/L, 100μg/L,.200μg/L, 400μg/L, 600μg/L, 800μg/L, 1000μg/L
Degree series calibration solution.
7.4.4 The internal standard standard solution can be added directly to the calibration solution, or it can be added automatically by a peristaltic pump before the sample is nebulized.
7.4.5 The concentration range of the calibration solution can be adjusted according to the actual concentration of the element to be measured in the sample.
7.5 Determination
7.5.1 Instrument Preparation
After igniting the plasma, set the optimal working conditions according to the instrument instruction manual. Use the mass spectrometer tuning solution to adjust the sensitivity of the instrument,
Oxide, double charge, resolution and other indicators, after meeting the requirements, sample injection and determination.
7.5.2 Plotting the calibration curve
After the instrument meets the requirements, measure the calibration solution in turn. Taking the ratio of the element signal to be measured to the internal standard signal as the ordinate, the corresponding element
The mass concentration (μg/L) is the abscissa, draw the calibration curve and calculate the regression equation, the correlation coefficient should not be less than 0.995.
7.5.3 Determination of sample
The test conditions are the same as 7.5.1.Before each sample measurement, flush the system with nitric acid solution until the signal is stable. When the sample is measured, it should be added with the calibration
Standard curve with the same amount of internal standard solution. Each sample was measured twice in parallel, and the arithmetic mean was taken as the measurement result. If the element to be tested is
If the content exceeds the range of the calibration curve, it should be re-measured after diluting with nitric acid solution (199), and record the dilution factor (f). sample solution present
When the polyatomic ion interferes, it can be corrected by collision mode according to the recommended conditions of the instrument.
Simultaneously measure the blank test solution.
8 Result calculation
The content of the element to be tested in the sample is calculated by mass concentration (ρ), the value is expressed in micrograms per liter (μg/L), and calculated according to formula (1).
9 Tolerance
Take the arithmetic mean of the parallel determination results as the determination result, and the relative standard deviation of the parallel determination results should meet the requirements of Table 1.
10 Interference and cancellation
10.1 Isobaric interference. elements with different atomic numbers and the same atomic mass have the same mass-to-charge ratio, which cannot be effectively resolved by mass spectrometers.
May cause serious interference. It can be corrected by selecting the appropriate isotope of the element to be measured, or using the calibration formula.
10.2 Interference of the more abundant isotopes on adjacent elements. the more abundant isotopes will produce tailing peaks, which will affect the measurement of adjacent mass peaks.
Certainly. The resolution of the m...