Spike Recovery Check

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Spike Recovery Check

Check

Parameters

oAdditional Notes for Parameters

Rules

Calculations

Associations

Sample Relationships

Errors

Exceptions

 

The DQM Check for Spike Recovery will qualify results if spike sample recoveries fall outside Quality Control (QC) limits.

 

Notes:

The QC_SPIKE_RECOVERY column or both of the QC_SPIKE_ADDED and QC_SPIKE_MEASURED columns must be populated in DT_RESULT_QC for this check to function.

For duplicate samples, the above columns or QC_DUP_SPIKE_RECOVERY column or both of the QC_DUP_SPIKE_ADDED and QC_DUP_SPIKE_MEASURED columns can be used.

Control limits for this check are determined as described in the RT_DQM_CONTROL_LIMITS section of the DQM_CONTROL_LIMITS help article.

 

Check

 

Check name is EarthSoft.DQM.SpikeRecovery2 = "Spike Recovery - Multiple Rules".

 

Parameters

 

This check uses four Global Parameters:

1.msd_parent_sample_ms See Sample Relationships section below for additional information.

2.reportable_result DT_RESULT.REPORTABLE_RESULT values to include in DQM datasets.

3.result_type_code DT_RESULT.RESULT_TYPE_CODE to include in DQM datasets.

4.test_type_batch – AT_TEST_BATCH_ASSIGN.TEST_BATCH_TYPE to include in DQM dataset.

 

Eleven parameters are available for this check.  None of these parameters allow for input of analyte-specific or method-specific PARAM_VALUEs.

1.Multiplier – Defaults to 4.

2.result_type_code_spike – Defaults to “SC”.

3.sample_type_blank_spike – Defaults to “BS,BD”.

4.sample_type_matrix_spike – Defaults to “FS,MS,MSD,SD”.

5.compare_to_calculated_LCS – Defaults to “N”.

6.compare_to_calculated_MS – Defaults to “N”.

7.acceptable_variance_LCS – Defaults to 1.

8.acceptable_variance_MS – Defaults to 1.

9.calculated_before_reported_LCS – Defaults to “N”.

10.calculated_before_reported_MS – Defaults to “N”.

11.dilution_factor_control_limit Control limit for comparison of each result's dilution factor. Results with a dilution factor over the control limit will not be evaluated. Defaults to 5.

 

 

Additional Notes for Parameters

 

1.If compare_to_calculated = "Y" or calculated_before_reported = "Y" then a Spike Recovery will be calculated for every spike compound using the data populated in the qc_spike_added and qc_spike_measured columns.

2.If compare_to_calculated = "Y" then

a.DQM will compare the calculated recovery to the recovery populated in the QC_RECOVERY column.

b.DQM will create an error message in the Errors tab if the difference between the calculated recovery and the reported recovery exceeds the acceptable_variance.

3.If calculated_before_reported = "Y" then

a.DQM will use the calculated value to compare to the Control Limit.

b.If the calculated value is not available, DQM will use the reported recovery value to compare to the Control Limit.

c.If the Control Limit is exceeded, an Exception will be added to the Exceptions table.

 

Notes:

Default parameter values listed above refer to the value provided in the DQM Starter QAPP.xlsx.

If there is no value for LOW_CUTOFF, then LOW_CUTOFF is set to zero and the third rule in each foursome of rules below is effectively eliminated.

For Matrix Spike and Matrix Spike Duplicate samples, RT_ANALYTE.ORGANIC_YN is required. If not populated, the result will be skipped.

 

Rules

 

There are twelve rules:

 

Rule #

Result Types

Rule Description

DQM Rule

1

Blank Spikes

% Recovery > Upper Cut Off

BLANK SPIKE > UPPER_CUTOFF

2

% Recovery > Upper Control Limit (UCL)

BLANK SPIKE > UCL

3

Lower Control Limit (LCL) > % Recovery ≥ Low Cutoff

LCL > BLANK > LOW_CUTOFF

4

% Recovery < Low_Cutoff

BLANK SPIKE < LOW_CUTOFF

5

Inorganic Spikes

% Recovery > Upper Cut Off

INORGANIC SPIKE > UPPER_CUTOFF

6

% Recovery > UCL

INORGANIC SPIKE > UCL

7

LCL > % Recovery ≥ Low_Cutoff

LCL > INORG > LOW_CUTOFF

8

% Recovery ≤ Low_Cutoff

INORGANIC SPIKE < LOW_CUTOFF

9

Organic Spikes

% Recovery > Upper Cut Off

ORGANIC SPIKE > UPPER_CUTOFF

10

% Recovery > UCL

ORGANIC SPIKE > UCL

11

LCL > % Recovery ≥ Low_Cutoff

LCL > ORG > LOW_CUTOFF

12

% Recovery < Low_Cutoff

ORGANIC SPIKE < LOW_CUTOFF

 

Additional Notes for the Result Types:

 

Blank Spikes – Review results with:

DT_SAMPLE.SAMPLE_TYPE_CODE = sample_type_blank_spike, and

DT_RESULT.RESULT_TYPE_CODE = result_type_code_spike.

Inorganic Spikes – Review results with:

DT_SAMPLE.SAMPLE_TYPE_CODE = sample_type_matrix_spike,

DT_RESULT.RESULT_TYPE_CODE = result_type_code_spike, and

RT_ANALYTE.ORGANIC_YN = 'N'.

Organic Spikes – Review results with:

DT_SAMPLE.SAMPLE_TYPE_CODE = sample_type_matrix_spike,

DT_RESULT.RESULT_TYPE_CODE = result_type_code_spike, and

RT_ANALYTE.ORGANIC_YN = 'Y'.

 

Use of Reason Codes with the rules is discussed here.

 

Calculations (where table is not indicated, it is DT_RESULT_QC)

 

Notes: For the calculations below and for DQM Version 7.21.1 and earlier versions, ALL fields mentioned in the RT_DQM_CONTROL_LIMITS must be populated and numeric or the DT_RESULT_QC or default value will be used as specified below. For example, if only RT_DQM_CONTROL_LIMITS.LCS_REC_LOWER_CUTOFF is populated for the Blank Spike, the default value of 0 will be used for the spike_lco.

 

RT_DQM_CONTROL_LIMITS is discussed in more detail here.

If QC_ORIGINAL_CONC > multiplier * QC_SPIKE_ADDED, then skip result.

If QC_SPIKE_RECOVERY is Numeric,

then spikeRecovery = QC_SPIKE_RECOVERY

else spikeRecovery for blank spikes = 100 * QC_SPIKE_MEASURED / QC_SPIKE_ADDED and for matrix spikes = 100 * ((QC_SPIKE_MEASURED-QC_ORIGINAL_CONC) / QC_SPIKE_ADDED)

For Spike Duplicates, if regular columns are NULL, then if QC_DUP_SPIKE_RECOVERY is Numeric,

then spikeRecovery = QC_DUP_SPIKE_RECOVERY

else spikeRecovery for blank spike duplicate = 100 * QC_DUP_SPIKE_MEASURED / QC_DUP_SPIKE_ADDED and for matrix spike duplicate = ((QC_DUP_SPIKE_MEASURED-QC_ORIGINAL_CONC) / QC_DUP_SPIKE_ADDED)

 

For Blank Spikes:

 

If any of the below values are numeric, the following RT_DQM_CONTROL_LIMIT fields will be used:

spike_lco = RT_DQM_CONTROL_LIMITS.LCS_REC_LOWER_CUTOFF

spike_lcl = RT_DQM_CONTROL_LIMITS.LCS_RECOVERY_LCL

spike_ucl = RT_DQM_CONTROL_LIMITS. LCS_RECOVERY_UCL

spike_upper_cutoff = RT_DQM_CONTROL_LIMITS. LCS_REC_UPPER_CUTOFF

 

When the value above is not populated:

spike_lco = 0.0

spike_lcl = QC_SPIKE_LCL

spike_ucl = QC_SPIKE_UCL

spike_upper_cutoff = 999.99

 

For Matrix Spikes (Inorganic and Organic):

 

If any of the below are numeric, the following RT_DQM_CONTROL_LIMIT fields will be used:

spike_lco = RT_DQM_CONTROL_LIMITS.MS_REC_LOWER_CUTOFF

spike_lcl = RT_DQM_CONTROL_LIMITS.MS_RECOVERY_LCL

spike_ucl = RT_DQM_CONTROL_LIMITS.MS_RECOVERY_UCL

spike_upper_cutoff = RT_DQM_CONTROL_LIMITS.MS_REC_UPPER_CUTOFF

 

When the value above is not populated:

spike_lco = 0.0

spike_lcl = QC_SPIKE_LCL

spike_ucl = QC_SPIKE_UCL

spike_upper_cutoff = 999.99

 

Associations

 

For Blank Spikes, associated results are found using TEST_BATCH_ID.

For Matrix Spike and Matrix Spike Duplicate samples (Inorganic or Organic), associated results are found using the PARENT_SAMPLE_CODEs based on the Global Parameter parameter setting msd_parent_sample_ms.

 

Sample Relationships

 

When the global parameter msd_parent_sample_ms = “Y”.

oThe PARENT_SAMPLE_CODE for Matrix Spike Duplicate (MSD) sample should match the Matrix Spike (MS) SYS_SAMPLE_CODE.

oThe PARENT_SAMPLE_CODE for the MS sample should match the original sample’s SYS_SAMPLE_CODE.
Although the parent for MSD samples are MS, the result populated in DT_RESUL_QC.QC_DUP_ORIGINAL_CONC should equal the original sample’s result value.

When the global parameter msd_parent_sample_ms = “N”.

oThe PARENT_SAMPLE_CODE for both the MSD and MS should match the original sample’s SYS_SAMPLE_CODE.

 

Exceptions (see Calculations for definitions):

 

If spikeRecovery < spike_lco, then qualify spike result and any associated result.

If spike_lcl > spikeRecovery ≥ spike_lco, then qualify spike result and any associated result.

oIf spikeRecovery > spike_ucl, then qualify spike result and any associated result with a detected concentration.

 

An example remark saved to DT_RESULT_DQM_REMARK for an exception is:

"Associated Result from : The Blank Spike Recovery is less than the Lower Cutoff."

 

Errors

 
Where table is not indicated, it is DT_RESULT_QC.

If QC_SPIKE_RECOVERY, QC_SPIKE_ADDED, and QC_SPIKE_MEASURED are all NULL or Not Numeric, then add error and skip result.

If QC_SPIKE_RECOVERY is NULL or Not Numeric, and either QC_SPIKE_ADDED or QC_SPIKE_MEASURED are also NULL or Not Numeric, then add error and skip result.

For Spike Duplicates, if regular columns are NULL, apply the same error checking to QC_DUP_SPIKE_RECOVERY, QC_DUP_SPIKE_ADDED, and QC_DUP_SPIKE_MEASURED.

If the Upper Control Limit is NULL or Not Numeric in both RT_DQM_CONTROL_LIMITS and DT_RESULT_QC, then add error and skip result.

If the Lower Control Limit is NULL or Not Numeric in both RT_DQM_CONTROL_LIMITS and DT_RESULT_QC, then add error and skip result.

If compare_to_calculated = Y and the variance between the reported and calculated recoveries exceed the acceptable_variance, then add error and skip result

If ORIGINAL_CONC exceeds multiplier * QC_SPIKE_ADDED, then add warning and skip result.

Dilution Factor exceeded the Dilution Factor Control Limit.

 

Example error messages:

"One of the required rules for this check is not present in the RT_DQM_RULE table."
       If you receive this error, the QAPP can be updated following the How to Update Existing QAPPs documentation page.

“Spike Duplicate Recovery data missing from DT_RESULT_QC for either {QC_SPIKE_RECOVERY} or {QC_SPIKE_ADDED} and {QC_SPIKE_MEASURED}.”  

“The variance between the reported (90) and the calculated (100) Spike Recovery exceeded the Acceptable Variance (2). at sys_sample_code=BS_1_AQ_UCO_TEST and analytic_method='SW8260' and cas_rn='100-41-4'”

“Matrix Spike Recovery Check - Skipped Because Original Concentration exceeds Multiplier * Spike Added at sys_sample_code=MSD_2_SOL_UCO_TEST and analytic_method='SW8270' and cas_rn='86-73-7'”

"Spike Recovery {FIELDNAME} is missing or not numeric;_".

This check was skipped for TEST_ID = '2622720'  because the Dilution Factor (10) exceeded the Dilution Factor Control Limit (5)