WorkflowRefining & Petrochemicals

Certificate of Analysis Review

Certificate of analysis review that reads each certificate against its lab record, its contract and the tank it describes, and holds the one that passes every limit for the wrong reason.

Follow one diesel tank from 10:42 to 10:50 ↓
The problem

A certificate of analysis can pass every limit after the tank has changed

The lab system compares each result with its limit, and when every line passes the certificate goes out. Nobody opens the movements record unless something already looks wrong. If rundown went into the tank after the sample was drawn, the paper still reads clean.

The other traps are quieter. One result sits just under the limit, inside the spread the lab itself states for the test. Another was typed in again after a retest. Some lines have no test behind them, or the lab ran a good method the contract does not name. With twenty-odd certificates a day, the one that matters looks like the rest.

Built forProduct quality chemistsLab supervisorsTank farm schedulersProduct tradersInternal auditors

The Problem Today

Checks stop at the limits, so a certificate can pass every line after its sample stops describing the tank.

15 ppm
the sulfur limit: a tank just under it reads as a plain pass published
2,350
hours a year to check 9,400 certificates at 15 minutes each our estimate

Cross-checked by hand today

  • Certificate
  • Lab results
  • Tank gauges
  • Contracts
  • Product in after the sampleA limit check cannot see the movements record
  • Blanks that read as a passA line typed in with no test behind it

The Solution

  1. Each line on one rulerResult, limit, method and test band, tied to the lab record
  2. One time line of the tankReceipts, mixing, sample and certificate, from gauges and movements
  3. Checks limits cannot makeSample, method and history: agents hold and explain, with sources
  4. Two people decideThe chemist proposes; the lab supervisor opens the records and signs

Built-in controls

  • A second person opens the records, then signs
  • Agents never release or change a result
  • A hold blocks each start request until signed

What You Get

Quality teams catch the doubtful tank before the vessel loads, and routine grades clear in a sampled batch.

  • An evidence file per decisionWho proposed, what they opened, who signed
  • Holds that block start requestsBerth, rack and rail requests wait for a signature
  • Routine grades in one sign-offNear-limit and flagged lines stay out of the batch
One certificate, minute by minute

Eight minutes on one certificate of analysis that passed every line

A diesel tank is due to load a tanker at 14:00. Its certificate went out at 10:05 with every limit passed, and the agents held it at 10:07. Here is what the chemist, the lab supervisor and the scheduler did next.

demoThe refinery, the vessel, the buyer, the people and each result are sample data, and the limits are a sample contract.

  1. 0110:42

    Fifteen lines inside their limits, and the certificate is held

    Product quality chemist

    Each line sits on one ruler between its limits, with the method and the test band the lab states. Sulfur reads 14.6 against a maximum of 15, shaded near the edge. Below the ruler runs one time line of the tank, and on it a red bar: 4,100 barrels from Unit 23 after the sample was drawn.

  2. 0210:43

    Sulfur 14.6 from two runs, inside a band of 1 ppm

    Product quality chemist

    She opens the sulfur line. Two runs, 14.5 and 14.7, by ultraviolet fluorescence on one instrument. The lab states its own test band as plus or minus 1 ppm, a sample value. So the tank could read 15.6 in another lab. The result passes, and it is also the kind of pass a buyer's lab can overturn.

  3. 0310:44

    At 07:30 the rundown swung into the tank, after the 06:10 sample

    Product quality chemist

    The movement order tells it plainly. Tank 309 hit high level at 07:25, and Unit 23 diesel rundown went to Tank 307 from 07:30 until 09:55. The sample was drawn at 06:10. Nothing on the certificate shows it, because the lab system never reads the movements record.

  4. 0410:44

    Last 20 certificates on this tank read 6.9 to 10.8 ppm

    Product quality chemist

    The tank screen puts the level, the movements and the history together. This tank's median is 8.6, so 14.6 is odd as well as near the limit. The agent shows how the heel and the fill reach that reading from the analyzer, and labels it a sum, never a result.

  5. 0510:45

    Reject and resample, in her own words, and she cannot sign it

    Product quality chemist

    She proposes rejecting the certificate under reason code S-1, product entered the tank after sampling, and writes why: the rundown came in after the sample, so close the inlet, mix and resample. The sign button stays off for her. Whoever proposes a decision does not sign it, so it waits for the lab supervisor.

  6. 0610:47

    The gauge goes from 151,800 to 155,900 barrels after the sample

    Lab supervisor

    Before he can sign, he has to open the records the hold rests on himself. He reads the movement order, then the gauge readings: 151,800 barrels when the sample was drawn, 155,900 after the receipt. Her opens do not count for him; the product records his own, on the trail.

  7. 0710:48

    Rejected: the certificate is void and a resample is ordered

    Lab supervisor

    He gives his reason and signs. The certificate is void. A resample order goes out, the tank stays closed to receipts, and the time line now shows mixers planned, a resample at 14:30 and an earliest loading of 17:00. The agents found it and held it. Only he could reject it.

  8. 0810:50

    A start request for the berth is refused, with the reason

    Tank farm scheduler

    She asks for the tanker's start. Refused, with the reason: certificate void, resample ordered, a person has to decide. Her resample plan lists the steps, with the inspector's shore sample moved to 14:30 and loading 3 hours late. No valve moves from here; the product blocks the request and the board operator stays in charge.

  9. 0910:50

    Who opened what, minute by minute, before anyone signed

    Internal auditor

    The trail reads from the bottom up: the chemist opened the sulfur line and the movement order, then proposed; the supervisor opened the movement order and the gauge, then rejected with his words; the scheduler's start was refused. Each certificate has an evidence file built from the same rows.

The tank's night and morning, record by record

Every row comes from a system the lab never reads when it issues a certificate.

WhenWhat happenedRecord
Until 01:40Unit 23 rundown fills the tank from 12,500 to 151,800 barrelsMovements
01:45 to 04:45Mixers run 3 hours, then the tank settlesMovements
06:10Upper, middle, lower and composite samples drawnSample log
07:30 to 09:55Rundown swung in when the next tank hit high level: 4,100 barrelsMovement order and gauge
09:48Sulfur approved: runs 14.5 and 14.7, result 14.6 mg/kgLab system
10:05Certificate issued; all 15 lines with a limit passCertificate
10:07Agents hold it and tell the shift supervisor about Unit 23Hold

demoSample data, from the working solution. Under this site's own rule, anything entering a tank between its sample and loading voids the certificate.

Four more held this morning, each passing its limits

Today's list holds 23 certificates. The agents held these besides the diesel tank.

Typed differently from the lab record

A gasoline certificate prints 212 °F at 50% recovered; the lab system holds 221. Both driveability indexes are inside the limit.

A line with no test behind it

Hydrogen sulfide on a molten sulfur certificate was filled in with no result in the lab system.

A method the paper does not name

Jet fuel freezing point ran on automatic method B. The pipeline's paper names the manual method or automatic method A.

Odd for this coke lot

A petroleum coke result falls outside the lot's history, so a person reads it before the rail cars move.

demoSample data, from the working solution.

Around the lab

The certificate of analysis refinery list, holds and rules

Six screens the lab, the tank farm and audit use around the same morning.

Today's 2316 clear, 4 held, 1 rejected, 2 still in the lab, sorted by what stops next. Released by agents: 0.
Line by lineThe certificate as issued beside what the lab system holds. Two lines do not match: 50% recovered, and the driveability index worked from it.
Methods against the paperWhat the lab ran against what the paper names. Where the paper names no method, the row says not checked rather than match.
Near a limitLines within the lab's stated test band of a limit. Each leaves the routine batch and is signed one by one. The band never passes or fails anything.
Holds and clocksEach hold with its clock and what it blocks. A question to the shift supervisor asks for Unit 23 to be looked at before the next tank is sampled.
The site ruleA receipt after the sample voids the certificate: this site's own rule, signed by the lab supervisor. A change takes two people and applies to later checks.

demoSample data, from the working solution.

The agents

Seven agents on each certificate, and none of them may release it

They hold and explain. People decide.

Certificate reader

Reads the issued certificate line by line and ties each value to its place.

  • Never fills a blank; a line with no value is reported
Lab record matcher

Matches each line to the approved lab result, method, instrument, analyst and time.

  • Never picks between two results; reports both
Specification checker

Compares results with the specification, and methods with the contract's quality clause.

  • Never interprets a clause; a difference goes to a person
Precision checker

Finds results within the lab's stated test band of a limit.

  • Never calls a line pass or fail on the band
Sample checker

Reads gauging, movements, mixers and the sample log to ask whether the sample still describes the tank.

  • Never estimates its way to a pass
  • An online analyzer is never a result
History checker

Compares each result with this tank's or grade's last certificates.

  • Never explains a cause it cannot cite
Hold writer

Writes the hold in plain words, with sources and options, and builds the evidence file.

  • Never releases, signs or changes a result

Releasing a cargo stays with the lab supervisor

What the product will not do on its own, however clean the certificate looks.

No release by an agentAgents hold and explain. A chemist proposes, and the lab supervisor signs after opening the records.
The proposer is never the signerThe proposer cannot sign. Where the supervisor ran a test himself, the lab manager signs instead.
No valve movesA hold blocks the start request to the terminal and refuses a rundown swing into the tank. The board operator moves product.
An estimate is never a resultThe analyzer and the mixing sum show the records agree. Only a lab test counts.
Release and safety questions go to a personQuestions about release, loading or safety go to a named person, with no data sent back.

What quality managers ask about certificate of analysis review

What is a certificate of analysis for a refinery product?

A certificate of analysis lists each test on a tank, batch or lot with its result, method and limit, and it is what lets a refinery ship. This review reads each certificate of analysis against the lab record, the specification, the contract and the tank's own movements before anyone signs.

Our lab system already checks results against limits. What does this add?

The checks a limit cannot make: whether the sample still describes the tank, whether the method is the one the contract names, whether a result is odd for this tank, and whether a line has a test behind it at all.

Is a certificate of quality for fuel handled the same way?

Yes. Whatever the site calls the paper, each line is tied to its lab record, and the tank's gauging, movements and sample log are read beside it.

How do you read a certificate of analysis that is near a limit?

Against the test band the lab states for that test. A result within the band of a limit is taken out of the routine batch and signed one by one, and the band never passes or fails the line by itself.

Does a hold stop the tank?

It blocks every start request for that tank to the terminal, the rack and rail, and refuses a rundown swing into it, until a person signs. The product moves no valve; the board operator does.

Can routine grades still go out quickly?

Routine rack and rail certificates with no flag go in a batch. The lab supervisor opens a random sample before signing, and each certificate in the batch says on its record whether he opened it.

Whose rule says a receipt after sampling voids the certificate?

The site's own, set by the lab and signed by the lab supervisor. Each customer sets its own rules, limits and test bands, and loads its own specifications and contracts.

Bring a week of
your certificates.

We will read them against your lab records, contracts and tank movements and show you which ones we would have held.