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Summary of ASTM D4628

This standard test method describes procedures for analyzing barium, calcium, magnesium, and zinc in unused lubricating oils using atomic absorption spectrophotometry. Key steps include weighing oil samples into bottles, adding a base oil and potassium suppressant solution, then analyzing by atomic absorption spectrophotometry at specific wavelengths for each element. Working standards are also prepared from stock standard blends diluted with base oil for calibration purposes. The method is suitable for determining low levels of the specified elements in unused lubricating oils.

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370 views6 pages

Summary of ASTM D4628

This standard test method describes procedures for analyzing barium, calcium, magnesium, and zinc in unused lubricating oils using atomic absorption spectrophotometry. Key steps include weighing oil samples into bottles, adding a base oil and potassium suppressant solution, then analyzing by atomic absorption spectrophotometry at specific wavelengths for each element. Working standards are also prepared from stock standard blends diluted with base oil for calibration purposes. The method is suitable for determining low levels of the specified elements in unused lubricating oils.

Uploaded by

Dewi Wulandhari
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as XLSX, PDF, TXT or read online on Scribd
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ASTM D-4628

Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic

Summary

NO Tools
1 Atomic Absorption Spectrophotometer
2 Analytical Balance
Automatic Measuring Pipet or Volumetric Class A Pipet, 50-mL
capacity

3 Bottles with Screw Caps, 60 mL (2 oz)

Shaker, Mechanical Stirrer, or Ultrasonic Bath, capable of


4 handling 60-mL bottles
5

Sample Preparation

NO Barium, Calcium, Magnesium, Zinc


Weigh the sample to three significant figures into a 60-mL (2-oz)
1 bottle. The sample mass is chosen to give an absorbance
reading of 0.2 to 0.5.

2 Add base oil to make 0.25 ±0.01 g total mass.

Add 50 mL of potassium suppressant solution and dissolve

The maximum sample size to be used is 0.25 g, and the


3 minimum is 0.05 g.
To hazy samples add 0.25 6 0.01 mL of 2-ethyl hexanoic acid
and shake. If this clears up the haze, the analysis is run, and the
4 dilution error is corrected by multiplying the found results by
1.005.
If the sample remains hazy, the sample is not suitable to be
5 analyzed by thistest method.
Samples yielding absorbances greater than 0.5 even with the
6 minimum sample size can be accurately diluted with new base
oil to a suitable concentration.
Aspirate the sample solution and determine the absorbance,
7 aspirating solvent alone before and after each reading.

Inject the samples for Barium,Calcium, Magnesium, and Zinc


8 determination by Acetylene/nitrous oxide flame AAS
Analytical Line

Barium : 553.6 nm
Calcium : 422.7 nm
Magnesium : 285.2 nm
Zinc : 213.9 nm
m, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry

Notes Materials
Base Oil, metal-free
2-Ethyl Hexanoic Acid
Kerosine, Metal-Free

Suitable volumetric flasks or plastic bottles may be Oil-Soluble Metal Compounds


substituted

Potassium Ionization Suppressant Solution


Working Standards

QC Sample

alcium, Magnesium, Zinc


Timbang sampel ke dalam botol 60 mL (Massa sampel
dipilih untuk memberikan pembacaan absorbansi 0,2
sampai 0,5)
Tambahkan Base Oil untuk membuat total massa 0.25
±0.01 g
Tambahkan 50 mL Potassium Ionization Suppressant
Solution
Ukuran sampel maksimal adalah 0.25 g dan minimal
0.05 g.
Untuk sampel yang haze, tambahkan 0.25 ± 0.01 mL
2-ethylhexanoic acid lalu shake. Jika tidak dapat
membersihkan haze, analisis dapat dilakukan dengan
faktor koreksi, mengalikan hasil dengan 1.005
Jika sampel tetap haze, sampel tidak cocok untuk
dianalisis dengan metode pengujian ini.
Sampel yang menghasilkan absorbansi lebih besar dari
0,5 dengan ukuran sampel minimal boleh diencerkan
dengan base oil baru (homogen).
Aspirasikan sampel dan tentukan absorbansi, untuk
pelarut aspirasikan sebelum dan sesudah pembacaan.
Injek sampel untuk analisis Barium, Kalsium,
Magnesium, dan Seng pada AAS Flame dengan
asetilen/nitrous oxide
Notes
Viscosity of about 4 cSt at 100°C Conostan Oil Based Metal Free
Free of interfering metals

stock standard blend in base oil Conostan Oil Based with Metal Compounds

containing an oil-soluble potassium compound in


kerosine at 2.0 ± 0.1 g potassium/litre of solution

portions of one or more liquid petroleum materials


that are stable and representative of the samples of
interest

Working Standards

Working Standards Preparations


Weighing into six 60-mL bottles 0.25, 0.20, 0.15,
0.10, 0.05, and 0 g of stock standard blend (Oil-
Soluble Metal Compounds)
add 0.0, 0.05, 0.10, 0.15, 0.20, and 0.25 ±0.01 g of
base oil, respectively.
Add 50 mL of potassium ionization suppressant
solution to each bottle and shake or stir to dissolve.

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