2014 GNF Sampling and Analysis Protocol for Ontario Regulation 300/14 made under the Nutrient Management Act, 2002

Table of Contents

  1. Introduction
  2. Sampling Methods and Locations for Soils In Situ
  3. Sampling Methods and Locations for GNF
  4. Laboratory Analysis and Data Quality Requirements
  5. GLOSSARY

1.0 Introduction

The GNF Sampling and Analysis Protocol (the "S&A Protocol") sets out methods required for sampling and analysis of GNF and soil as required by O. Reg. 300/14 (the Regulation) made under the Nutrient Management Act, 2002 ("NMA"). This S&A Protocol sets out sampling and analysis requirements that are complementary to and in addition to those set out in the Regulation.

The Regulation sets out what materials need to be sampled and analyzed, how frequently they need to be sampled and analyzed, and which parameters need to be measured.

The requirements of the S&A Protocol form part of the Regulation and are legally enforceable. Anyone reading this Protocol should ensure that they have the most recent version of the Regulation, the Greenhouse Nutrient Feedwater Management Protocol and this Protocol.

Any term used in the S&A Protocol that is defined in the Regulation or the NMA has the same meaning as in the Regulation or the NMA. In addition, any reference to GNF includes a mixture resulting from the mixing of GNF with other GNF or with liquid agricultural source materials as permitted under the Regulation unless otherwise indicated in this Protocol.

2.0 Sampling Methods and Locations for Soils In Situ

A controller of an agricultural operation at which soil samples are taken for the purpose of the Regulation shall ensure that the rules in this section are complied with.

2.1 Collection of Soil Samples

Soil samples must be collected in order to provide a small volume of soil for analysis that is representative of the whole volume of soil within the GNF application area. There are a number of different ways to comply with this requirement. This section describes the minimum sampling requirements.

To be representative of the GNF application area, the sample must be comprised of a number of sub-samples as explained below. The sub-samples must include the depth of soil that would normally be tilled which in most cases is approximately 15 centimeters (6 inches).

2.2 Number of Soil Sub-Samples for Analysis

Sub-samples must be collected to provide an accurate composite soil sample. The minimum required number of sub-samples for different sizes of GNF application areas are outlined below.

For a GNF application area of 5 or fewer hectares:

  • collect a minimum of twenty sub-samples.

For a GNF application area of more than 5 hectares:

  • collect at least two additional sub-samples for each additional hectare over 5 hectares to a maximum of 40 sub-samples.

All sub-samples must be mixed together thoroughly to produce the composite sample that is to be submitted for analysis.

3.0 Sampling Methods and Locations for GNF

A controller of an agricultural operation shall ensure when sampling GNF that the rules in this section are complied with.

3.1 GNF Sampling Equipment and Methods

When taking a sample from a permanent GNF storage facility, you must use the bucket toss method or the dipper method as described below in sections 3.1.1 and 3.1.2.

For sampling from permanent GNF storage facilities, take at least the number of sub-samples required by section 3.3 from different locations of the storage facility and combine these sub-samples into a larger container (composite) where they must be mixed thoroughly (homogenised). This composite sample must then be transferred to a clean sample bottle for shipment to the laboratory for analysis.

For sampling from GNF transfer systems, the sample must not be taken during the start-up or shut-down of the GNF transfer system. A number of sub samples must be taken and be combined together.

3.1.1 Bucket-Toss

Attach a rope to a small plastic bucket and then throw the bucket out into the facility, let it sink and then carefully pull the bucket back.

Swirl the bucket and then pour about 1 litre of the contents into a second clean plastic bucket. Repeat this from different locations around the perimeter of the facility until at least the required number of sub-samples under section 3.3 has been taken.

3.1.2 Dipper

Tape a clean plastic wide-mouth bottle (250-1000 ml capacity) securely to a pole that is long enough to reach over any scum collected at the edge of the facility. Remove, at least, the number of sub-samples required by section 3.3 and pour them into a clean plastic bucket. Once all of the sub-samples have been taken, mix the bucket contents and transfer to sample bottles for analysis.

3.2. Requirements for Agitation

If agitation is required by the Regulation it must be carried out using a mechanical mixing device, aeration device or using a hauling truck's pumping system. It must provide a well-mixed material for sampling.

3.3 Number of GNF Sub-Samples for Analysis

A minimum of five sub-samples must be collected and composited for each sample. The number of sub-samples required is based on the volume to be removed for land application. Table 1 sets out the minimum number of sub-samples required per composite sample. Where the volume of GNF removed for land application in Column 1 applies, the minimum number of sub-samples opposite it in Column 2 must be taken.

Composites must be well-mixed (homogenized) and transferred to properly labelled laboratory bottle(s). Information concerning the sample volume required, the type of sample bottles to be used and the appropriate preservative needed, based on the analytical test(s) required must be obtained from the person operating the laboratory.

Table 1. Minimum Number of GNF Sub-Samples per Composite for Different Land Application Volumes
Column 1: Volume to be Removed for Land Application Column 2: Minimum Number of Sub-Samples per Composite
Less than 1,000 m3 5
1,000 m3 to 10,000 m3 10
Greater than 10,000 m3 15

4.0 Laboratory Analysis and Data Quality Requirements

The person operating a laboratory at which an analysis is performed for the purposes of this Regulation shall ensure that the following requirements are complied with.

For each parameter in Column 1 of Table 2, the Matrix (Column 2), Reporting Detection Limit (RDL) (Column 3) and Acceptable Reference Methods (Column 4) opposite the parameter applies.

Despite the above paragraph, analytical methods that are the equivalent to the acceptable reference methods may also be used. An analytical method is equivalent if the laboratory possesses data that confirms the method produces equivalent test results, including method detection limits (MDLs) equal to or lower than the Reporting Detection Limit (RDL) in Table 2.

Guidance for calculating the laboratory MDL, quality control practices and method principles is available in the Sampling and Analysis Protocol for Ontario Regulation 267/03 Made under the Nutrient Management Act, 2002.

Table 2. Laboratory Analysis
Column 1: Parameter Column 2: Matrix Column 3: RDL Column 4: Acceptable Reference Methods
Phosphorus (P) Soil Not applicable OMAFRA P
Potassium (K) Soil Not applicable OMAFRA Cations
Regulated Metals (Trace Metals):
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Lead (Pb)
Molybdenum (Mo)
Nickel (Ni)
Zinc (Zn)
Soil µg/g

1
12
2.5
10
10
2.5
5.0
25
MOECC E3470
USEPA 3050B/3051A
USEPA 6010C/6020A
Modified USEPA SW-846/3050B/3052/200.7 ICP-OES
Regulated Metals:
Mercury (Hg)
Soil 0.05 µg/g MOECC E3059
APHA/AWWA/WEF 3030G
APHA/AWWA/WEF 3112B
Modified USEPA 3005/7471/SM3112B Cold vapour
USEPA 3005
Regulated Metals:
(Hydride Metals):
Arsenic (As)
Selenium (Se)
Soil µg/g

1.4
1
MOECC E3245
MOECC E3470 (digestion)
USEPA 3050B/3051A
USEPA 7062/7742
Modified USEPA SW-846/3052/200.7 ICP-OES
USEPA 3005
Total Solids GNF 50 mg/L MOECC 3188
Modified EPA 160.2
Gravimetric
Recommended Methods of Manure Analysis, University of Minnesota A3769
Ammonia + Ammonium Nitrogen GNF 0.01 mg/L USEPA 350.1 or 350.2
MOECC E3364
APHA 4500-NH3 H (mod)
Nitrate + Nitrite Nitrogen GNF 0.04 mg/L MOECC E3364
USEPA 353.2
APHA 4500-NO3 D (mod)
APHA 4500-NO3 F and NO2-N (USEPA 353.2 (mod)
Regulated Metals:
(Trace Metals): Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Lead (Pb)
Molybdenum (Mo)
Nickel (Ni)
Zinc (Zn)
GNF mg/L

0.003
0.2
0.03
0.10
0.015
0.005
0.01
0.5
MOECC E3094 MOECC E3071
USEPA 3005A/3010A/3015A
USEPA 6010C/6020A
APHA/AWWA/WEF 3030F
APHA/AWWA/WEF 3120
Modified USEPA SW-846/200.7/200.8 ICP-OES
APHA 3120 (mod)
Regulated Metals:
Mercury (Hg)
GNF
0.5 µg/L
MOECC E3058
MOECC E3060
MOECC E3526USEPA 245.7
USEPA 245.7/1631E/3005
APHA/AWWA/WEF 3112B
Regulated Metals:
(Hydride Metals): Arsenic (As)
Selenium (Se)
GNF mg/L

0.01 0.005
MOECC E3091
USEPA 3005A/3010A/3015A
USEPA 7062/7742
APHA/AWWA/WEF 3030F APHA/AWWA/WEF 3114
APHA 3120B (mod)
Additional Elements:
Boron (B)
Sodium (Na)
Potassium (K)
Phosphorus (P)
GNF mg/L

0.05 0.5 0.05 0.1
MOECC 3094
MOECC 3071
MOECC 3470
USEPA 3005A/3010A/3015A
USEPA 6010C/6020A
APHA/AWWA/WEF 3030F
APHA/AWWA/WEF 3120
APHA/AWWA/WEF 3030B
APHA/AWWA/WEF 3030 K
APHA/AWWA/WEF 3120B
3030B: dissolved
3030K: total
3120B: ICP-OES
AOCA 985.01
Direct reading ICP-OES
USEPA 6010C (mod)
Total Kjeldahl Nitrogen (TKN) GNF/liquid ASM mixtures only 0.05 mg/L MOECC E3516
Modified SM 4500-N C Colorimetric
USEPA 351.2

APHA/AWWA/WEF: American Public Health Association / American Water Works Association / Water Environmental Federation "Standard Methods"

ICP-OES: inductively coupled plasma optical emission spectrometry

Note: Reference methods are available from the following sources:

5.0 GLOSSARY

Ammonium Nitrogen: Means ammonia nitrogen plus ammonium nitrogen.

Composite Sample: A sample that is made up of a number of sub-samples that have been thoroughly mixed together.

Matrix: Any type of material, e.g., soil, GNF

Sub-sample: A single sample taken directly from the material being sampled or a portion of a composite sample.


For more information:
Toll Free: 1-877-424-1300
E-mail: ag.info.omafra@ontario.ca
Author: OMAFRA Staff
Creation Date: 15 December 2014
Last Reviewed: 15 December 2014