GB/T 28159-2025 (GB/T 28159-2011) PDF English
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 31.030
L 90
Electronic grade phosphoric acid
Issued on: DECEMBER 30, 2011
Implemented on: JULY 01, 2012
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Product categories... 5
4 Requirements... 5
5 Test methods... 6
5.1 Safety instructions... 6
5.2 General provisions... 6
5.3 Appearance... 6
5.4 Phosphoric acid content... 6
5.5 Readily oxidizable substance content... 7
5.6 Metal ion content... 7
5.7 Anion content... 10
5.8 Particle measurement... 15
6 Inspection rules... 15
6.1 Batching and sampling... 15
6.2 Inspection items... 16
7 Marking, labeling... 16
8 Packaging, transportation, storage and handling... 17
Appendix A (informative) Instrument working conditions... 18
Appendix B (informative) Ion chromatogram... 20
Electronic grade phosphoric acid
1 Scope
This Standard specifies the requirements, test methods, inspection rules, as well as
marking, packaging, transportation, storage, etc. of electronic grade phosphoric acid.
This Standard applies to electronic grade phosphoric acid for industry use.
This Standard does not address safety issues in use. Users of this Standard are
responsible for establishing appropriate safety and health clauses and limitations on the
scope of use.
2 Normative references
The following documents are indispensable for the application of this document. For
dated references, only the edition cited applies. For undated references, the latest edition
of the referenced document (including any amendments) applies.
GB/T 191, Packaging - Pictorial marking for handling of goods
GB/T 601, Chemical reagent - Preparations of reference titration solutions
GB/T 603, Chemical reagent - Preparations of reagent solutions for use in test
methods
GB/T 1282-1996, Chemical reagent - Phosphoric acid
GB 3149-2004, Food additive - Phosphoric acid
GB/T 6678, General principles for sampling chemical products
GB/T 8170, Rules of rounding off for numerical values & expression and judgment
of limiting values
GB/T 11446.1, Electronic Grade Water
GB 15258, General rules for preparation of precautionary label for chemicals
GB 50472, Code for design of electronic industry clean room
spectrometer separates the ions according to the mass-to-charge ratio and quantifies the
content of the corresponding ions in the sample by the intensity of the ion mass
spectrum peak.
Use the standard addition method for sample analysis, and the linear range of the
standard curve is 20 ng/L ~ 500 ng/L.
5.6.2 Reagents and materials
5.6.2.1 Nitric acid. Ultrapure nitric acid with a metal ion content not exceeding 1 μg/L,
or a certified standard solution of the corresponding concentration.
5.6.2.2 Nitric acid solution (1+19, volume ratio). Take 150 mL of nitric acid as specified
in 5.6.2.1 and add it to 950 mL of ultrapure water.
5.6.2.3 Tuning solution. 1 μg/L, provided by the instrument supplier or a certified
tuning solution.
5.6.2.4 Tuning working solution. Take 20 mL of the tuning solution specified in 5.6.2.3
and place it in a clean polytetrafluoroethylene bottle. This solution can be kept for 7
days if refrigerated at 4 ℃ and used repeatedly.
5.6.2.5 Multi-element standard stock solution. Select the standard solution with a
known metal ion concentration of 100 μg/mL listed in Table 1, or select a certified
standard solution of other concentrations.
5.6.2.6 Multi-element standard working solution. Take 100 μL of the standard stock
solution specified in 5.6.2.5 and place it in a clean polytetrafluoroethylene bottle; add
2 mL of nitric acid specified in 5.6.2.1; use ultrapure water to dilute to 100 mL; shake
well. The metal ion concentration in this standard working solution is 100 μg/L. This
solution can be kept for 7 days if refrigerated at 4 ℃ and used repeatedly.
5.6.2.7 High-purity argon, hydrogen, helium and other gases required by the instrument
shall have a purity of not less than 99.995%.
5.6.2.8 Phosphoric acid standard sample (quality control sample). 1% phosphoric acid
standard solution. Select a certified phosphoric acid standard solution or a quality
control sample approved by inter-laboratory comparison.
5.6.3 Instruments and apparatuses
5.6.3.1 Inductively coupled plasma-mass spectrometer (ICP-MS), equipped with
Collision Reaction System (ORS) (recommended instrument detection limit. low-mass
elements (Be) < 5 × 10-9, medium- and high-mass elements (In, Bi) < 1 × 10-9; abundance
sensitivity. low-mass elements ≤ 1 × 10-6, high-mass elements ≤ 5 × 10-7; stability.
short-term RSD ≤ 4% (20 min), long-term RSD ≤ 5% (2 h), 24-hour mass axis deviation
±0.1 amu; anti-interference capability. oxide ratio ≤ 3%, double charge ratio ≤ 8%.)
5.6.3.2 Precision sampling gun. 100 μL, 1 000 μL, 5 mL.
5.6.3.3 Ultrapure water purifier, with a 0.1 μm terminal filter, for online preparation of
ultrapure water with a purity of not less than 18.2 MΩ·cm (25 °C).
5.6.4 Analysis steps
5.6.4.1 Sample test fluid
Weigh 10 g of the sample to be tested in batches to an accuracy of 0.000 2 g; place them
in six 100 mL high-purity polytetrafluoroethylene bottles; add 2 mL of ultrapure nitric
acid; then add 0 mL, 0.1 mL, 0.2 mL, 0.4 mL, 0.6 mL, and 1.0 mL of the multi-element
standard working solution specified in 5.6.2.6 in that order; use ultrapure water to dilute
to 100.00 g; shake well.
5.6.4.2 Blank test solution
Add 2 mL of ultrapure nitric acid to a polytetrafluoroethylene high-purity bottle; use
ultrapure water to dilute to 100 mL (100.00 g); shake well.
All utensils and sampling gun tips must be soaked in high-purity nitric acid solution
that meets the requirements of 5.6.2.2 for 24 hours, rinsed repeatedly with ultrapure
water and dried before use.
5.6.4.3 Determination
Adjust the instrument working conditions and use the tuning working solution specified
in 5.6.2.4 to adjust the instrument measurement parameters. The tuning shall meet the
instrument working requirements. Select the mass number of the element to be
measured. The selection of the isotope of the element to be measured shall be based on
the possible interference in the sample matrix. Select a suitable gas mode with less
interference and determine the isotope with higher abundance. With the response value
of the analytical peak as the ordinate and the amount of standard solution of the element
to be measured as the abscissa, use the chemical workstation equipped with the
instrument (random chromatography software) to draw a standard curve for the test
results. The content corresponding to the distance between the intersection of the
standard curve on the horizontal axis and the origin is the content of the element to be
measured in the sample test solution. This is then used to calculate the content of the
element to be measured in the sample.
Carry out a blank test under the same analytical conditions; deduct blank interference
according to the operating requirements of the instrument manual.
The linear correlation coefficient of the standard curve shall not be lower than 0.995.If
the measurement result exceeds the linear range, the test solution shall be re-prepared
or the sample concentration shall be changed and re-measured.
Note. When adjusting the instrument, it is advisable to give priority to comparative
determination of phosphoric acid standard samples that meet the
requirements of 5.6.2.8.The absolute difference between the determination
results of the main elements and the known concentrations should not exceed
a certain percentage limit (relative to the known concentration). Otherwise,
the instrument should be readjusted. If the concentration of an element is
known to be ≥1×10-7, the limit value is ≤10%; if the concentration of an
element is known to be 1×10-8 ~ 5×10-98, the limit value is ≤20%; if the
concentration of an element is known to be 1×10-9 ~ 1×10-8, the limit value is
≤30%.
5.6.5 Detection-limit, precision and recovery
5.6.5.1 Detection-limit (LOQ)
The detection-limit of various elements in 1%H3PO4 are shown in Table A.1 in
Appendix A.
5.6.5.2 Precision (RSD)
The absolute difference between two independent determination results obtained under
repeated conditions shall not exceed 30% of the arithmetic mean; the precision test data
of each element are shown in Appendix A Table A.2.
5.6.5.3 Recovery
The recovery of inductively coupled plasma-mass spectrometry shall be in the range of
75% ~ 125%; the test data of precision of each element are shown in Appendix A, Table
A.2.
5.7 Anion content
5.7.1 Volumetric method
Operated in accordance with the relevant requirements of GB/T 1282-1996, the
detection-limit shall be ρ(Cl-) 0.01 mg/L, w(NO- 3) 0.05 mg/kg, ρ(SO2- 4) 0.4 mg/L.
5.7.1.1 Chloride
5.7.1.1.1 Reagents and materials
a) Nitric acid. 1+1 solution;
b) Silver nitrate. 17 g/L solution;
c) Chloride standard solution [ρ(Cl-) = 1 000 mg/L]. select a certified standard
solution of corresponding concentration.
5.7.1.1.2 Analysis steps
Leave the solutions prepared according to a) and b) for 10 min. The turbidity of the
solutions shall not be greater than that of the corresponding standard comparison
solutions.
5.7.2 Ion chromatography (quantitative method)
5.7.2.1 Principle of the method
The ion chromatograph uses a sample loop tube for fixed volume injection. The sample
solution passes through a dedicated ion suppression column, and the trace impurity
anions are separated from the phosphoric acid using an ion exclusion column. The
separated and collected components are then concentrated through an ion exchange
concentration column and form a Gaussian distribution chromatographic peak in the
conductivity detector. The area (or peak height) of the chromatographic peak is
proportional to the concentration of the component. The integrator of the instrument
picks up this signal and gives the quantitative result of the component. The standard
addition method should be used to determine the impurity anions in the sample.
5.7.2.2 Reagents and materials
5.7.2.2.1 Anion standard working solution
Separately draw standard working solutions of chloride (Cl-), nitrate (NO- 3), and sulfate
(SO2- 4) to prepare mixed standard working solutions of ρ(Cl-)10 mg/L, ρ(NO- 3) 50 mg/L
and ρ(SO2- 4)100 mg/L. The appropriate concentration can be determined according to
the anion concentration in the sample.
5.7.2.2.2 Ion chromatography columns
Use ion chromatography columns supporting the instrument. guard column, analytical
column, C concentration column, capture column and exclusion column.
5.7.2.2.3 Eluent
Ultrapure water, 20 mmol/L ~ 60 mmol/L potassium hydroxide (preferably produced
by an eluent generator).
5.7.2.3 Equipment and instruments
Ion chromatograph, equipped with an automatic eluent generator, a conductivity
detector and a chromatography workstation, an automatic anion regeneration
suppressor, a concentration pump, and an external six-way valve. The instrument
detection limit is. 0.002 μg/mL for Cl-, 0.001 μg/mL for NO- 3 and SO2- 4.
5.7.2.4 Analysis steps
5.7.2.4.1 Ion chromatography conditions
6.1.2 Sampling should be carried out online at the sampling port of the packaging
machine on the production line. When sampling finished products, determine the
number of sampling unit in accordance with the provisions of GB/T 6678.Before
sampling, first confirm that the temperature of the product in the package is higher than
10 °C. Carry out sampling in a clean room at a room temperature of approximately
20 °C. The sampling method is to place the package in a Class 100 ultra-clean working
environment (laminar flow hood or clean room) specified in GB 50472 for no less than
30 minutes; allow it to stabilize; then open the lid for sampling. When sampling, use a
special clean sampler to insert it into the packaging barrel to three-quarters of the depth
of the material layer to take samples.
6.1.3 When the sample is not less than 100 g, mix the sample evenly and divide it into
two clean and dry high-purity polyethylene bottles or polytetrafluoroethylene bottles
and seal them. Affix a label to the bottle, indicating. manufacturer name, product name,
batch number, sampling date and name of the sampler (the label can be simplified if the
manufacturer samples the product itself). Use one bottle for testing and keep the other
for 3 months for future reference.
6.2 Inspection items
6.2.1 Factory inspection shall be carried out by the quality supervision and inspection
department of the manufacturer in accordance with the requirements of this Standard.
The manufacturer shall ensure that each batch of products leaving the factory complies
with the requirements of this Standard.
6.2.2 When any of the following situations occurs, carry out type inspection.
a) When there are major changes in raw materials, processes, or equipment;
b) When resuming production after a long-term shutdown;
c) When the quality supervision department makes a request.
7 Marking, labeling
7.1 The packaging drums of electronic grade phosphoric acid shall be firmly and clearly
marked with the following information. manufacturer’s name and address, product
name “electronic grade phosphoric acid”, production license number, net weight, batch
number or production date, number of this standard, and the “corrosive article” mark
specified in GB/T 191 and GB 15258.The label format shall comply with the provisions
of GB 15258.
7.2 Each batch of electronic grade phosphoric acid shipped out of the factory shall be
accompanied by a quality certificate. The contents shall include. manufacturer name,
product name, net weight, batch number or production date, certification that the
product quality complies with this Standard and a reference to this Standard.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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