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D5600-22 – Standard Test Method Technical Guide
📜 Scope and Significance
This test method, designated D5600‑22, is intended for the determination of trace metals in test specimens of raw and calcined petroleum coke using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP‑AES). The presence and concentration of metallic elements play a critical role in determining the suitability of petroleum coke for various end uses. The method is applicable only to samples containing less than one mass percent ash, and elements present at concentrations above the upper working range can be determined with additional dilutions.
The method covers commonly determined trace metals, with detection limits and optimum ranges varying based on sample matrices and spectrometer model. The values stated in SI units are to be regarded as the standard.
⚙️ Test Procedure
A representative gross sample, prepared according to Practice D346, is ashed at 700 °C. The ash is fused with lithium borate and the melt is dissolved in dilute hydrochloric acid (HCl). The solution is then introduced into an ICP‑AES instrument by free aspiration or an optional peristaltic pump for simultaneous or sequential multielemental determination. Concentrations are calculated by comparing emission intensities from the sample with those from calibration standards.
Below is a summary of key test parameters:
| 🔬 Parameter | 📏 Specification |
|---|---|
| Test Material | Raw and Calcined Petroleum Coke |
| Maximum Ash Content | < 1 mass % |
| Ashing Temperature | 700 °C |
| Fusion Agent | Lithium Borate |
| Dissolution Acid | Dilute Hydrochloric Acid (HCl) |
| Analysis Method | ICP‑AES |
| Sample Introduction | Free Aspiration or Peristaltic Pump |
💡 Tip: This method is only valid for samples with less than 1 mass % ash. For higher‑ash cokes, alternative test methods should be considered.
📊 Analytical Considerations and Quality
The ICP‑AES method allows for robust multielemental analysis. For quality assurance, the test method must be applied in accordance with Practices D6299 and D7260 for optimization, calibration, and validation. Detection limits and working ranges for each element are detailed in Table 1 of the standard. Consistent sample preparation, including sieving per Specification E11, is essential for reproducibility.
Contamination control and the use of reagent water conforming to Specification D1193 are critical to obtaining reliable results.
✅ Dilution: If an element’s concentration exceeds the upper limit of the working range, the solution can be re‑analyzed after an appropriate dilution to bring it within the calibrated range.
❓ Frequently Asked Questions
🔍 What is the principle of this test method?
The petroleum coke sample is ashed at 700 °C, fused with lithium borate, dissolved in dilute HCl, and analyzed by ICP‑AES to determine trace metal concentrations.
💡 What elements can be analyzed using this method?
This method covers commonly determined trace metals, which are listed in Table 1 of the standard. Typical analytes include vanadium, nickel, iron, and sodium.
⚡ What is the ash content limitation?
The method is applicable only to samples with less than 1 mass % ash. Samples exceeding this limit may require alternative approaches.
📌 How are samples prepared for analysis?
Samples are collected and crushed following Practice D346, then sieved. A gross sample is ashed, fused with lithium borate, dissolved in HCl, and aspirated into the ICP‑AES instrument.