GB/T 32812-2016 PDF English
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Metal working fluid - Limit requirements and determination methods of hazardous substance
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GB/T 32812-2016: PDF in English (GBT 32812-2016) GB/T 32812-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 75.140
E 49
Metal working fluid - Limit requirements and
determination methods of hazardous substance
ISSUED ON: AUGUST 29, 2016
IMPLEMENTED ON: MARCH 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 List and limit requirements of prohibited substances ... 5
5 Determination methods of prohibited substances ... 6
6 List of controlled substances ... 7
Appendix A (Normative) Determination of nonylphenol polyoxyethylene ether -
liquid chromatography ... 8
Appendix B (Normative) Determination of C10~C13 short-chain chlorinated
paraffin content - gas chromatography ... 11
Appendix C (Normative) Determination of polycyclic aromatic hydrocarbons in
metal working fluid - liquid chromatography ... 14
Appendix D (Normative) Determination of diethanolamine content - gas
chromatography ... 19
Bibliography ... 22
Metal working fluid - Limit requirements and
determination methods of hazardous substance
1 Scope
This Standard specifies the list, limit requirements and determination methods
of prohibited substances in metal working fluid, and list of controlled substances;
but currently does not specify the requirements for restricted substances.
This Standard applies to metal working fluids produced and sold.
2 Normative references
The following documents are indispensable for the application of this document.
For the dated references, only the editions with the dates indicated are
applicable to this document. For the undated references, the latest edition
(including all the amendments) are applicable to this document.
GB/T 4756 Method for manual sampling of petroleum liquids
GB/T 28612-2012 Green manufacturing of mechanical products -
Terminology
SN/T 2704.3 Cutting fluid and machining process waste fluid - Part 3:
Determination of nitrite - Ion chromatography
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Metal working fluid
The medium used for lubrication, cooling, rust prevention and cleaning of
metals and their alloys in the cutting and forming process.
Note: It is divided into water-based metal working fluid, oil-based metal working fluid. The
form includes liquid, semi-fluid or solid.
3.2
Note 3: Prohibited substances include but are not limited to the above substances.
5 Determination methods of prohibited substances
5.1 Sampling
Sampling of metal working fluid shall be carried out in accordance with the
provisions of GB/T 4756.
5.2 Nitrite NO2-
The content of nitrite in the metal working fluid is determined using nitrite NO2-
test paper. The arbitration test is carried out in accordance with SN/T 2704.3.
5.3 Nonylphenol polyoxyethylene ether
See Appendix A for the determination of nonylphenol polyoxyethylene ether
content in metal working fluids.
5.4 Short-chain chlorinated paraffin
See Appendix B for the determination of short-chain chlorinated paraffin content
in metal working fluids.
5.5 Polycyclic aromatic hydrocarbons
See Appendix C for the determination of the content of polycyclic aromatic
hydrocarbons in metal working fluids.
5.6 Diethanolamine
See Appendix D for the determination of diethanolamine content in metal
working fluids.
5.7 Lead
The determination of lead content in metal working fluid is carried out according
to the following steps:
a) TAKE 1 g of sample in a porcelain crucible; HEAT and carbonize it on an
electric hot plate; ADD 2 mL of concentrated nitric acid and 5 drops of
concentrated sulfuric acid; carefully heat until the white fume is exhausted;
MOVE it into a 550 °C high-temperature furnace for ashing (6 h~8 h);
b) TAKE it out after cooling; ADD 1 mL of nitric acid (1+1) solution; HEAT to
dissolve the ash. If the ash of the sample is not completely dissolved, add
1 mL of mixed acid (nitric acid : perchloric acid=9 : 1) solution; HEAT to
Appendix A
(Normative)
Determination of nonylphenol polyoxyethylene ether - liquid
chromatography
A.1 Overview
This appendix specifies the liquid chromatography detection method for
nonylphenol polyoxyethylene ether (n=2~10) in water-based metal working
fluids.
A.2 Method
After taking 1 g of sample and adding 10 mL of ethanol for extraction, the
ethanol extract is determined by liquid chromatography and quantified by
external standard method.
A.3 Reagents and standard solutions
Reagent and standard solution requirements:
- Methanol (HPLC grade);
- Acetonitrile (HPLC grade);
- Ethanol (analytical purity);
- Pure water; the resistivity is greater than 18.2 MΩ • cm;
- Nonylphenol polyoxyethylene ether standard; average degree of
polymerization n=9; purity is ≥99%;
- Nonylphenol polyoxyethylene ether standard solutions: Accurately weigh
an appropriate amount of nonylphenol polyoxyethylene ether; USE
methanol to dilute; prepare a series of standard working solutions of the
required concentration 10 mg/L, 50 mg/L, 100 mg/L, 200 mg/ L and 500
mg/L.
A.4 Apparatus
Test apparatus and related requirements:
- High performance liquid chromatograph, equipped with fluorescence
Appendix B
(Normative)
Determination of C10~C13 short-chain chlorinated paraffin content - gas
chromatography
B.1 Overview
This appendix specifies the detection method for the content of C10~C13 short-
chain chlorinated paraffins in the metal working fluid with a concentration (mass
fraction) ranging from 0.1%~2.5%.
B.2 Method
TAKE 0.2 g of sample and add 10 mL of n-heptane to dilute or extract; then take
the diluent or extract into the gas chromatograph with ECD detector for analysis.
B.3 Reagents and materials
Reagent and material requirements:
- N-heptane; the purity is not less than 99%;
- C10~C13 chlorinated paraffin standard; the purity is not less than 99%;
- C10~C13 chlorinated paraffin n-heptane standard solution: WEIGH an
appropriate amount of C10~C13 chlorinated paraffin standard; USE n-
heptane as the dilution solvent; prepare C10~C13 chlorinated paraffin n-
heptane standard solutions with concentrations of 20 mg/L, 50 mg/L, 100
mg/L, 200 mg/L and 500 mg/L, respectively.
B.4 Apparatus
Test apparatus and related requirements:
- Gas chromatograph, equipped with electron capture detector (ECD) and
automatic injection device;
- Pipette, 1 mL;
- Measuring cylinder, 10 mL;
- Glass sample bottles with screw caps, 1.5 mL and 25 mL;
- Microinjector, 10 μL or higher accuracy;
Appendix C
(Normative)
Determination of polycyclic aromatic hydrocarbons in metal working
fluid - liquid chromatography
C.1 Overview
This appendix specifies the liquid chromatography detection method for the
content of polycyclic aromatic hydrocarbons (PAHs) and benzopyrene (BaP) in
metal working fluids.
C.2 Method
After the sample is diluted or extracted by n-heptane, it is determined by a high
performance liquid chromatograph equipped with a polar chromatographic
column and a differential refractive index detector; quantified by the external
standard method. The total content of polycyclic aromatic hydrocarbons is the
mass sum of bicyclic aromatic hydrocarbons and above-tricyclic aromatic
hydrocarbons.
C.3 Reagents and standard solutions
Reagent and standard solution requirements:
- Cyclohexane (analytical pure), without benzene;
- N-heptane (HPLC grade), as the mobile phase;
- O-xylene (analytical purity); the purity is greater than 98%;
- Hexamethylbenzene; the purity is greater than 98%;
- Naphthalene; the purity is greater than 98%;
- Dibenzothiophene; the purity is greater than 95%;
- 9-methylanthracene; the purity is greater than 95%;
- Fluorene; the purity is greater than 98%;
- Phenanthrene; the purity is greater than 98%;
- Benzopyrene; the purity is greater than 98%;
Accurately weigh 1 g of metal working fluid sample into a 25 mL glass sample
bottle with a screw cap; ADD 10 mL of n-heptane; carry out dilution or ultrasonic
extraction for 30 min. After standing for 30 min, transfer the n-heptane diluent
or extract to a 1.5 mL sample bottle for instrumental analysis.
C.5.2 Liquid chromatographic analysis conditions
Typical liquid chromatographic analysis conditions are as follows. Other
chromatographic columns and analysis conditions, which can achieve the same
separation effect, can also be used:
- Serial chromatographic columns: one NH2 column (150 mm×4.6 mm×5 μm)
and one SB-CN column (150 mm×4.6 mm×5 μm);
- Chromatographic column temperature: 35 °C;
- Mobile phase: n-heptane;
- Refractive index range of the differential refractive index detector is 1.3~1.6;
- Flow rate: 1.0 mL/min;
- Injection volume: 10 μL.
C.5.3 Sample determination
C.5.3.1 Determination of content of polycyclic aromatic hydrocarbons
The mixed calibration solutions A to D of polycyclic aromatic hydrocarbons are
determined sequentially. According to the chromatographic peak area and the
corresponding concentration, establish a standard working curve. According to
the retention time of o-xylene, fluorene and phenanthrene, determine the
integration domain of chromatographic peak of monocyclic aromatic
hydrocarbons, bicyclic aromatic hydrocarbons, tricyclic and above-tricyclic
aromatic hydrocarbons. And use the polycyclic aromatic hydrocarbon reference
solution SCS1 to verify and confirm. TAKE 10 μL of sample into liquid
chromatograph for determination. From the retention time and peak area of
bicyclic aromatic hydrocarbons, tricyclic and above-tricyclic aromatic
hydrocarbons, the corresponding content of polycyclic aromatic hydrocarbons
can be obtained from the standard working curve.
C.5.3.2 Determination of benzopyrene content
First, the benzopyrene series standard working solutions are determined
sequentially from dilute to concentrated. According to the chromatographic
peak area and the corresponding concentration, establish a standard working
curve. TAKE 10 μL of sample into liquid chromatograph for determination. From
Appendix D
(Normative)
Determination of diethanolamine content - gas chromatography
D.1 Overview
This appendix specifies the detection method for diethanolamine content in
water-based metal working fluids with a concentration (mass fraction) ranging
from 0.1%~2%. Samples with diethanolamine content (mass fraction) higher
than 2% can be tested after being diluted with ethanol.
D.2 Method
After the metal working fluid is extracted using ethanol, it is analyzed by gas
chromatograph.
D.3 Reagents and materials
Reagent and material requirements:
- Diethanolamine; the purity is not less than 99%;
- Ethanol, analytically pure;
- Preparation of the standard stock solution of diethanolamine: Accurately
weigh 0.5 g of diethanolamine into a 100 mL volumetric flask; USE ethanol
to dilute to the mark and mix well. The concentration of the standard stock
solution is 5000 mg/L;
- Diethanolamine standard working solutions: PIPETTE an appropriate
amount of standard stock solution and use ethanol to dilute, to prepare
concentrations of 100 mg/L, 200 mg/L, 500 mg/L, 1000 mg/L and 2000
mg/L, respectively.
D.4 Apparatus
Test apparatus and related requirements:
- Gas chromatograph, equipped with FID detector and automatic injection
device;
- Ultrasonic cleaner;
- Pipette, 1 mL;
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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