GB/T 41330-2022 PDF English
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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)
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GB/T 41330-2022: PDF in English (GBT 41330-2022) GB/T 41330-2022
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.060.50;71.040.40
CCS G 76
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)
(ISO 17294-2:2016, Water quality -- Application of inductively coupled plasma
mass spectrometry (ICP-MS) -- Part 2: Determination of selected elements
including uranium isotopes, NEQ)
ISSUED ON: MARCH 9, 2022
IMPLEMENTED ON: OCTOBER 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and Definitions ... 5
4 Method summary ... 5
5 Reagents or materials ... 5
6 Instruments and equipment ... 7
7 Test steps ... 7
8 Calculation of the result ... 10
9 Tolerance ... 10
10 Interference and cancellation ... 11
11 Safety matters ... 11
Appendix A (Informative) Selection of the internal standard substances ... 13
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)
Warning -- The strong acids used in this document are corrosive, avoid inhalation
or contact with skin. If being splashed, rinse immediately with plenty of water and
seek medical attention immediately in severe cases.
1 Scope
This document describes the determination of trace copper, iron, sodium, calcium, and
magnesium content in water used in boiler and cooling systems by inductively coupled
plasma mass spectrometry.
This document is applicable to the determination of trace copper, iron, sodium, calcium,
and magnesium content in water used in boiler and cooling systems. Measurement
range: copper content 0.1 µg/L~1000 µg/L, iron content 5 µg/L~1000 µg/L, sodium
content 10 µg/L~1000 µg/L, calcium content 10 µg/L~1000 µg/L, magnesium content
1 µg/L~ 1000 µg/L; when the content exceeds 1000 µg/L, it shall be diluted and then
measured.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 602 Chemical reagent -- Preparations of standard solutions for impurity
GB/T 6041 General rules for mass spectrometric analysis
GB/T 6907 Analysis of water used in boiler and cooling system -- Sampling method
of water
GB/T 33087-2016 Ultra pure water for instrumental analysis specification and test
methods
commercially available standard solutions.
5.9 Copper standard stock solution II: 100 mg/L.
5.10 Iron standard stock solution I: 1000 mg/L. Weigh 1.000 g of metallic iron, and the
weight shall be accurate to 0.2 mg. Add it to 100 mL hydrochloric acid solution, and
heat the solution until the metallic iron all dissolves; cool the solution and transfer it to
a 1000 mL volumetric flask; dilute it with water to the mark. Or use commercially
available standard solutions.
5.11 Iron standard stock solution II: 100 mg/L.
5.12 Sodium standard stock solution I: 1000 mg/L. Weigh 2.542 g standard sodium
chloride that has been pre-burned to a constant amount at 500 °C~600 °C, and the
weight shall be accurate to 0.2 mg; dissolve it in water and transfer to a 1000 mL
volumetric flask; dilute with water to the mark, and shake well. Or use commercially
available standard solutions.
5.13 Sodium standard stock solution II: 100 mg/L.
5.14 Calcium standard stock solution I: 1000 mg/L. Weigh 2.500 g of high-grade pure
calcium carbonate that has been pre-dried at 105 °C~110 °C to a constant amount, and
the weight shall be accurate to 0.2 mg. Place it in a 100 mL beaker, add 50 mL water
and 10 mL hydrochloric acid, then dissolve it and transfer to a 1000 mL volumetric
flask; dilute it with water to the mark, and shake well. Or use commercially available
standard solutions.
5.15 Calcium standard stock solution II: 100 mg/L.
5.16 Magnesium standard stock solution I: 1000 mg/L. Weigh 1.660 g of premium pure
magnesium oxide that has been pre-burned at 800 °C±50 °C to a constant amount, and
the weight shall be accurate to 0.2 mg. Place it in a 100 mL beaker, add a small amount
of water to wet the sample, and add 25 mL of hydrochloric acid; then, dissolve it and
transfer it to a 1000 mL volumetric flask; dilute it to the mark with water, and shake
well. Or use commercially available standard solutions.
5.17 Magnesium standard stock solution II: 100 mg/L.
5.18 Mixed standard stock solution: The certified mixed standard solution can be
purchased; or use the standard stock solution I or II of each element to prepare the
mixed standard stock by group according to the mutual interference between elements,
the properties of the standard solution and the content of the element to be measured.
Then, store the solutions in sealed polyethylene or polypropylene bottles.
5.19 Mixed standard solution: 10 mg/L. Pipette 10.00 mL copper, iron, sodium, calcium,
and magnesium standard stock solution II, put it in a 100 mL volumetric flask, and
dilute to the mark with a nitric acid solution (1+99); shake well. The solution shall be
prepared just before being used.
5.20 Internal-standard standard stock solution: 10 mg/L or 1 mg/L, commercially
available. 6Li, 45Sc, and 74Ge should be selected as internal standard elements. See
Appendix A for the selection of the internal standard corresponding to the mass number
of each element to be measured.
5.21 Internal-standard standard solution: According to the requirements of the
instrument manual, dilute the internal standard stock solution with a 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. Standard solutions containing
elements such as lithium (Li), yttrium (Y), beryllium (Be), magnesium (Mg), cobalt
(Co), indium (In), thallium (Tl), lead (Pb), and bismuth (Bi) should be selected and used
as the mass spectrometer tuning solutions.
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
a collision/reaction cell.
6.2 Digestion equipment: a temperature-controlled electric hot plate or a microwave
digestion apparatus or a graphite digestion apparatus.
6.3 Sampling bottle: The material shall be high-density polypropylene, high-density
polyethylene, or fluorinated polyethylene propylene (FEP). The material of the bottle
body and bottle cap shall not contain or leach any measured elements.
6.4 Beaker: The material shall be polytetrafluoroethylene, 100 mL or 250 mL.
6.5 Volumetric flask: The material shall be polypropylene, meltable
polytetrafluoroethylene (PFA), or quartz.
7 Test steps
7.1 General
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, place it in 8 volumetric
flasks with a volume of 100 mL, and dilute it to the mark with a nitric acid solution
(1+99); shake well to obtain the low concentration series calibration solutions, with the
concentrations of 0.0 µg/L, 5.0 µg/L, 10.0 µg/L, 20.0 µg/L, 40.0 µg/L, 60.0 µg/L, 80.0
µg/L, and 100.0 µg/L.
7.4.3 Pipette an appropriate amount of mixed standard solution, place it in 8 volumetric
flasks with a volume of 100 mL, and dilute it to the mark with a nitric acid solution
(1+99); shake well, and obtain the high concentration series calibration solution, with
the concentrations of 0 µg/L, 50 µg/L, 100 µg/L, 200 µg/L. L, 400 µg/L, 600 µg/L, 800
µg/L, and 1000 µg/L.
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 manual. Use the mass spectrometer tuning solution to adjust the indicators
of the instrument, such as the sensitivity, the oxide, the double charge, and the resolution;
after the requirements are met, inject the sample and determine it.
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, and the mass concentration (µg/L) of the corresponding element as the
abscissa, draw the calibration curve and calculate the regression equation; the
correlation coefficient shall not be less than 0.995.
7.5.3 Sample determination
The test conditions are the same as 7.5.1. Before the measurement of each sample, rinse
the system with a nitric acid solution until the signal is stable. When the sample is
measured, it shall be added with an internal standard solution, and the amount is the
same as the calibration Standard curve. Each sample shall be measured twice in parallel,
and take the arithmetic mean as the measurement result. If the content of the element to
10 Interference and cancellation
10.1 Isobaric interference: The elements with different atomic numbers and the same
atomic mass have the same mass-to-charge ratio, which cannot be effectively resolved
by a mass spectrometer. It may cause serious interference. It can be corrected by
selecting the appropriate isotope of the element to be measured, or by 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. The resolution of the mass spectrometer can be adjusted to reduce
this interference.
10.3 Polyatomic (molecular) ion interference: The interference caused by a polyatomic
ion consisting of two or three atoms and having the same mass-to-charge ratio as an
element to be measured. The interference of polyatomic (molecular) ions is largely
affected by the operating conditions of the instrument, which can be reduced by
adjusting the instrument parameters.
10.4 Physical interference: It includes the interference caused by the difference in
viscosity, surface tension, and total dissolved solids between the test sample and the
standard solution. Physical interferences can be corrected with internal standard
substances.
10.5 Matrix suppression (ionization interference): An increase in the concentration of
easily ionizable elements will increase the number of electrons and cause a transition
in plasma equilibrium; usually, it will reduce the analytical signal; the situation is called
matrix suppression. Matrix interferences can be corrected with the internal standard
method.
10.6 Memory interference: When samples or standards with large differences in
concentration are analyzed continuously, the element to be measured in the sample is
easy to deposit and to stay on the vacuum interface, spray chamber, and atomizer, which
will cause memory interference. The increase in the time for rinsing the instrument
between the tests of different samples will help to avoid such interferences.
11 Safety matters
11.1 An exhaust device shall be installed above the burner of the instrument.
11.2 Regularly check the pipeline to prevent gas leakage and strictly abide by the
relevant operating procedures.
11.3 Argon and helium are inert gases, when using them, pay attention to ventilation to
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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